A high-performance insoluble sulfur wet production system and method

Abstract

The present invention discloses a high-performance insoluble sulfur production system and method. The insoluble sulfur wet production system can be used to produce high-performance insoluble sulfur products through the combination of sulfur polymerization, quenching, crushing, aging, extraction, drying, oil filling and other units. The production system of the present invention is a liquid phase environment, which avoids safety problems such as system blockage and powder explosion caused by solid or powder material transportation. The production process has the characteristics of safety and reliability, simple equipment and operation, and obvious energy saving effect.

Description

Technical Field

[0001] The invention belongs to the technical field of petrochemical industry and relates to a high-performance insoluble sulfur wet 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. From the perspective of the international market, only a few countries and regions can produce insoluble sulfur. The main production methods of insoluble sulfur are low-temperature melting method and gasification method.

[0004] 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 disclosed in the patent is not suitable for the production of insoluble sulfur by low-temperature melting method.

[0005] 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.

[0006] The existing low-temperature melting method for rapid cooling of high-temperature sulfur mostly adopts intermittent cooling in a quenching tower. After cooling, the material is intermittently taken out from the bottom of the quenching tower and sent to an oven for drying. The dried solid is processed by mechanical crushing, and finally extracted and oil-filled to obtain an insoluble sulfur product. At present, the process is complicated, the operation process is intermittent, and the insoluble sulfur produced has poor thermal stability and low yield. Therefore, it is necessary to develop key equipment for the production of insoluble sulfur, shorten the process flow, and realize continuous operation of the production process. Summary of the invention

[0007] In view of the problems existing in the prior art, the present invention provides a wet production system and method for insoluble sulfur.

[0008] According to a first aspect of the present invention, the present invention provides a high-performance insoluble sulfur wet production system.

[0009] The insoluble sulfur wet production system of the present invention comprises a polymerization kettle, a quenching and crushing tower, a drying and maturing tank, a three-in-one machine and an oil-filled kettle and corresponding connecting pipelines; the feeding port of the polymerization kettle is connected with the sulfur feeding pipeline, and the discharging port of the polymerization kettle is connected with the feeding port of the quenching and crushing tower; the discharging port of the quenching and crushing tower is connected with the feeding port of the drying and maturing tank, the discharging port of the drying and maturing tank is connected with the feeding port of the three-in-one machine, the discharging port of the three-in-one machine is connected with the feeding port of the oil-filled kettle, and the discharging port of the oil-filled kettle is connected with the insoluble sulfur product pipeline.

[0010] Furthermore, the drying and maturing tank is provided with a solvent delivery feed port, and the solvent delivery feed port is connected with a solvent delivery pipe.

[0011] Furthermore, the three-in-one machine is provided with an extractant feed inlet and a filtrate outlet, the extractant feed inlet is connected with the extractant feed pipe, and the filtrate outlet is connected with the filtrate discharge pipe.

[0012] Furthermore, the polymerization kettle is used to heat ordinary sulfur to 250°C to 300°C and keep the temperature constant for 1h to 2h. The polymerization kettle can be a vertical jacketed heating stirring kettle, a horizontal open mill, etc.

[0013] Furthermore, the quenching and crushing tower is used to perform liquid phase quenching and liquid phase crushing on the high-temperature molten sulfur transported from the polymerization kettle to obtain sulfur powder slurry.

[0014] Furthermore, the quenching and pulverizing tower can adopt a conventional structure in the art. In the present invention, the quenching and pulverizing tower is preferably a continuous wet ball mill separation device.

[0015] Furthermore, the continuous wet ball mill separation equipment comprises a cylinder, the interior of the cylinder comprises a feeding section and a crushing section from top to bottom, and a first rotating shaft is provided at the center of the cylinder;

[0016] The feed section is located at the upper part of the ball mill separation equipment, and is provided with a liquid inlet, a material inlet and a material distributor;

[0017] The crushing section is located at the lower part of the ball mill separation equipment, a stirring rod and a crushing ball are arranged in the crushing section, and a graded discharge module is arranged at the bottom of the crushing section;

[0018] The grading discharging module comprises a grading mesh plate and a grading wheel; the grading mesh plate is a cylindrical structure, and the mesh plate top cover at the upper end thereof is fixedly connected to the first rotating shaft; the cylindrical wall of the grading mesh plate is provided with a plurality of first slits or first openings; the grading wheel is a cylindrical structure, and the cylindrical wall of the grading wheel is provided with a plurality of second slits or second openings, and the width of the second slits or second openings widens from the inner side of the cylindrical wall to the outer side; and the bottom of the grading wheel is provided with a discharging port.

[0019] Furthermore, the grading mesh plate is mounted outside the grading wheel and is coaxial (cocentric) with the first rotating shaft. The grading wheel is fixedly connected to the second rotating shaft. The mesh plate top cover of the grading mesh plate is fixedly connected to the first rotating shaft, and the grading mesh plate thus constitutes the rotating shaft of the crushing section (i.e., the lower section of the first rotating shaft), and the stirring rods are evenly distributed on the outer wall of the grading mesh plate cylinder.

[0020] Furthermore, the first slit width or the first opening diameter is smaller than the diameter of the crushing ball.

[0021] Furthermore, the wet ball mill separation equipment can be used to cool, mix, crush, and grade the materials or liquids entering the equipment. The ball mill separation equipment is preferably a cylindrical barrel structure.

[0022] Furthermore, the liquid inlet and the material inlet are located at the top or upper wall of the cylinder of the ball mill separation equipment, and the material distributor is located inside the cylinder. The material inlet is connected to the material distributor inlet through a pipeline.

[0023] Furthermore, the ball mill separation device further comprises a spiral blade, which is located above the crushing section and fixed on the first rotating shaft. The spiral blade can be a conventional structure in the art. For example, the outer diameter of the spiral blade gradually increases from top to bottom, and the outer diameter of the largest spiral blade is half of the inner diameter of the cylinder of the ball mill separation device. The area where the spiral blade is located constitutes a spiral section, which is located between the feeding section and the crushing section and is located in the middle of the ball mill separation device.

[0024] Furthermore, a motor is arranged outside the top of the quenching and crushing tower body, and the motor is fixedly connected to the first rotating shaft. The first rotating shaft runs through the feeding section, the spiral section and the crushing section. The spiral pieces and the stirring rods are evenly distributed on the first rotating shaft and are fixedly connected to the first rotating shaft; the crushing balls are bulked in the crushing section. The grading discharging module is located at the axis center of the crushing section.

[0025] Furthermore, there is a gap between the lower edge of the grading mesh plate and the bottom plate of the equipment, 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.

[0026] Furthermore, the width of the second slit or the diameter of the second opening on the wall of the grading wheel barrel widens from the inside to the outside (i.e., from the center of the circle to the circumference), and the width of the inner slit or the inner opening is 0.2 to 0.9 times the width of the outer slit or the outer opening. Specifically, the width of the inner slit or the opening diameter is generally 2 mm to 15 mm. A sealing cover is provided on the top of the grading wheel, and the sealing cover is used to block the material from entering the inside of the grading wheel from the top of the grading wheel. A discharge port is provided at the bottom of the grading wheel, and the discharge port is also used as a second rotating shaft. The second rotating shaft can be connected to the grading motor through a rotating belt. The grading mesh plate and the grading wheel can rotate under the drive of the first rotating shaft and the second rotating shaft, respectively.

[0027] Furthermore, in the grading screen, the width of the first slit or the diameter of the first opening provided on the wall of the grading screen is generally 0.5 to 0.8 times the diameter of the crushing ball. The first slit or the first opening provided on the wall of the grading screen is used as a channel for the crushed slurry.

[0028] Furthermore, a rotary quick connector is arranged at the lower end of the discharge port of the grading wheel, and the other end of the rotary quick connector is connected to the discharge pipe. The second rotating shaft passes through the bottom plate of the equipment and is connected to the grading motor through a rotating belt.

[0029] Furthermore, the grading mesh plate is used to isolate the crushing balls to prevent them from entering the grading discharge module, and the grading wheel is used to separate the material powder that meets the particle size requirements.

[0030] Furthermore, the material distributor may be a granulator, an extruder or an atomizer, etc. The material distributor is used to disperse the feed material in the ball mill separation equipment.

[0031] In the present invention, the drying and maturation tank is used to filter, dry, mature and store the slurry transported from the quenching and crushing tower to obtain a crude insoluble sulfur product; at the same time, a transport solvent is added into the drying and maturation tank, and the transport solvent is mixed with the crude insoluble sulfur product to obtain a fluidized crude insoluble sulfur solid-liquid mixture.

[0032] In the present invention, the three-in-one machine is used to filter, wash, extract and dry the fluidized crude insoluble sulfur solid-liquid mixture obtained in the drying and maturing tank to obtain dry high-performance insoluble sulfur.

[0033] The drying and maturing tank and the three-in-one machine can be a flat-bottom filter-washing and drying machine, a cone-barrel filter-washing and drying machine or a filter-washing and drying integrated device, preferably a filter-washing and drying integrated three-in-one device.

[0034] Furthermore, the integrated filtering, washing and drying equipment comprises:

[0035] 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;

[0036] The material inlet and outlet cylinder is horizontally arranged and communicated with the filter sleeve; the material inlet and outlet cylinder comprises a material inlet at the top, a material outlet at the bottom, and a material inlet and outlet jacket;

[0037] 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.

[0038] 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.

[0039] 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.

[0040] 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.

[0041] 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.

[0042] 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.

[0043] 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.

[0044] 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. The filtering, washing and drying equipment is composed of at least one filter sleeve and at least one material inlet and outlet cylinder.

[0045] 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.

[0046] 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.

[0047] 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.

[0048] 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.

[0049] Furthermore, the filter sleeve is used for filtering, washing and drying integrated equipment, solid-liquid separation and heating. The heating medium can be steam, thermal oil or thermal medium water.

[0050] Furthermore, the oil-filled kettle is used to crush the dry high-performance insoluble sulfur delivered by the three-in-one machine again and mix it with oil to obtain a high-performance oil-filled insoluble sulfur product. The oil-filled kettle can be a dry powder machine or a vertical ball mill.

[0051] According to a second aspect of the present invention, the present invention provides a high-performance insoluble sulfur wet production method, wherein the above-mentioned insoluble sulfur wet production system is used.

[0052] Specifically, the wet production method of insoluble sulfur of the present invention includes the following contents:

[0053] (1) Sulfur at 120°C to 130°C enters the polymerization kettle through a feed pipe, and is heated in the polymerization kettle to 250°C to 300°C to obtain high-temperature sulfur. The high-temperature sulfur is kept at a constant temperature of 250°C to 300°C in the polymerization kettle for 1h to 2h to obtain the first logistics;

[0054] (2) The first stream enters a quenching and crushing tower, where it is quenched by quenching water and crushed in the liquid phase to obtain a fluidized second stream with a particle size of 0.5 mm to 2 mm;

[0055] (3) The second stream enters the drying and aging tank and is first filtered to separate the quenching water, and then the crude insoluble sulfur is dried by hot air or vacuum. When the water content of the crude insoluble sulfur is less than 1wt%, the crude insoluble sulfur is aged. After the aging, a transport solvent is added to the drying and aging tank to fully mix the solvent with the aged crude insoluble sulfur to obtain a fluidized third stream;

[0056] (4) The third stream enters the three-in-one machine for filtration, washing, extraction and drying. After filtration, the third stream is added to the three-in-one machine for extraction agent. After 2 to 4 extractions, the soluble sulfur is separated and the insoluble sulfur is left in the three-in-one machine. After extraction, the insoluble sulfur is dried to obtain the fourth stream. The moisture content of the fourth stream is less than 0.5wt%;

[0057] (5) The fourth logistics enters the oil-filled kettle for further crushing to obtain insoluble sulfur, and after crushing, filler oil is added to obtain a high-performance insoluble sulfur oil-filled product after oil filling.

[0058] Furthermore, in step (1), the heating of sulfur in the polymerization reactor to a constant temperature can be a continuous operation or an intermittent operation.

[0059] Furthermore, the aging in step (3) can be carried out by hot air or constant temperature in a tank. The aging time is 24h~50h, and the aging temperature is 50℃~70℃. The delivery solvent is an extractant.

[0060] Furthermore, the extractant in step (4) is one of carbon disulfide, o-xylene or n-hexane.

[0061] Furthermore, after the fourth stream in step (5) is crushed again, the particle size of the obtained insoluble sulfur is generally about 100 mesh. During the oil filling process, the volume ratio of the insoluble sulfur to the filling oil is generally 3-4:1.

[0062] Compared with the prior art, the high-performance insoluble sulfur wet production system and method of the present invention has the following advantages:

[0063] 1. In the insoluble sulfur wet production system of the present invention, high-performance insoluble sulfur products are produced through sulfur polymerization, quenching, crushing, aging, extraction, drying, and oil filling processes. During the system production process, sulfur is transported by liquid phase, avoiding safety problems such as system blockage and powder explosion caused by solid or powder material transportation. The production process has the characteristics of safety and reliability, simple equipment and operation, low operating cost, and obvious energy-saving effect.

[0064] 2. In the continuous wet ball mill separation equipment provided by the present invention, the continuous operation process of high-temperature sulfur cooling, mixing and crushing is realized by means of material distributor distribution, wet spiral cloth and wet crushing, thereby improving the sulfur grinding effect and efficiency; the sulfur is distributed, crushed and graded discharging in the ball mill separation equipment, thereby realizing the direct conversion of sulfur into sulfur powder that meets the product particle size requirements, avoiding graded filtration of the discharging after grinding, and avoiding the system blockage problem caused by the material transportation of powder materials between the current grinder and the graded filter, simplifying the process flow, and improving the uniformity of sulfur powder particle size distribution.

[0065] 3. In the integrated filtering, washing and drying equipment provided by the present invention, sulfur powder can be filtered, washed and dried in the same equipment, avoiding possible system blockage and safety problems in the transfer and transportation of sulfur between different equipment. Compared with conventional flat plate filtering, washing and drying equipment, the filtering area is increased, and the stirring paddle is used for heating and drying, which improves the filtering efficiency and drying efficiency, thereby shortening the filtering time and drying time. BRIEF DESCRIPTION OF THE DRAWINGS

[0066] Figure 1 It is a schematic diagram of the high-performance insoluble sulfur wet production system of the present invention.

[0067] Figure 2 It is a structural schematic diagram of a continuous wet ball mill separation device of the present invention.

[0068] Figure 3 It is a structural schematic diagram of a grading screen plate in the continuous wet ball mill separation equipment of the present invention.

[0069] Figure 4 It is a schematic structural diagram of a classifying wheel in the continuous wet ball mill separation equipment of the present invention.

[0070] Figure 5 It is an axial view of the second slit of the classifying wheel in the continuous wet ball mill separation equipment of the present invention.

[0071] Figure 6 It is a cross-sectional view of the integrated filtering, washing and drying device of the present invention.

[0072] Figure 7 It is an axial view of the inner drum in the integrated filtering, washing and drying device of the present invention.

[0073] Figure 8 It is a schematic cross-sectional view of the integrated filtering, washing and drying device DD of the present invention.

[0074] In the figure, each number mark corresponds to the name of the component: 100-sulfur feed pipeline, 200-polymerization kettle, 300-quenching crushing tower, 400-drying and maturing tank, 500-three-in-one machine, 600-oil-filled kettle, 1-solvent delivery pipe, 2-extractant feed pipe, 3-filtrate discharge pipe, 4-product, 5-delivery solvent feed port, 6-extractant feed port, 7-filtrate outlet;

[0075] 301-material inlet, 302-material feed pipeline, 303-liquid inlet, 304-liquid feed pipeline, 305-motor, 306-material distributor, 307-rotating belt, 308-first rotating shaft, 309-spiral sheet, 310-stirring rod, 311-crushing ball, 312-grading mesh plate, 313-grading wheel, 314-discharging pipe, 315-rotating quick connector, 316-discharging port, 317-second slit or opening, 318-first slit or opening, 319-second rotating shaft, 320-mesh plate top cover, 321-grading motor, A-feeding section of ball mill separation equipment, B-spiral section of ball mill separation equipment, C-crushing section of ball mill separation equipment, D-grading wheel grading section, E-grading wheel sealing cover, F-grading wheel neck.

[0076] 410-rotating shaft, 411-motor, 412-rotating jacket shaft, 413-shaft outer cylinder, 414-shaft inner cylinder, 415-shaft heating medium inlet, 416-shaft heating medium outlet, 417-stirring paddle, 418-distribution branch pipe, 420-end face flange cover, 430-filter sleeve, 431-outer cylinder, 432-filtrate outlet, 433-inner cylinder, 434-filter screen, 435-inner cylinder jacket, 436-inner cylinder jacket heat medium inlet, 437-inner cylinder jacket heat medium outlet, 438-vacuum gas outlet, 440-material inlet and outlet, 441-material inlet, 442-material inlet and outlet of cylinder jacket, 443-jacket heating medium inlet, 444-material outlet, 445-jacket heating medium outlet. DETAILED DESCRIPTION

[0077] The present invention will be further described below by way of specific examples, but is not limited to the following examples.

[0078] Example 1

[0079] This embodiment describes the wet production system of the present invention in detail with reference to the accompanying drawings.

[0080] like Figure 1 As shown, the insoluble sulfur wet production system of the present invention comprises a polymerization kettle 200, a quenching crushing tower 300, a drying and maturing tank 400, a three-in-one machine 500, an oil-filled kettle 600 and corresponding connecting pipelines. The feed port of the polymerization kettle 200 is connected to the sulfur feed pipeline 100, and the discharge port of the polymerization kettle 200 is connected to the feed port of the quenching crushing tower 300; the discharge port of the quenching crushing tower 300 is connected to the feed port of the drying and maturing tank 400, the discharge port of the drying and maturing tank 400 is connected to the feed port of the three-in-one machine 500, the discharge port of the three-in-one machine 500 is connected to the feed port of the oil-filled kettle 600, and the discharge port of the oil-filled kettle 600 is connected to the insoluble sulfur product pipeline 4.

[0081] The drying and maturing tank 400 is provided with a solvent feeding port 5, which is connected to the solvent feeding pipe 1. The three-in-one machine 500 is provided with an extractant feeding port 6 and a filtrate outlet 7, which is connected to the extractant feeding pipe 2 and the filtrate outlet 7 is connected to the filtrate discharge pipe 3.

[0082] The quenching and crushing tower 300 is preferably a continuous wet ball mill separation device. The continuous wet ball mill separation device comprises a cylinder, the interior of the cylinder comprises a feeding section A and a crushing section C from top to bottom, and a first rotating shaft 308 is arranged at the center of the cylinder.

[0083] The feed section A is provided with a liquid inlet 304, a material inlet 302 and a material distributor 306. The crushing section C is located at the lower part of the ball mill separation device, and a stirring rod 310 and a crushing ball 311 are arranged in the crushing section C. A graded discharge module is arranged at the bottom of the crushing section C.

[0084] The grading discharging module includes a grading mesh plate 312 and a grading wheel 313. The grading mesh plate 312 is a cylindrical structure, and the mesh plate top cover 320 at the upper end thereof is fixedly connected to the first rotating shaft 308; the cylindrical wall of the grading mesh plate 312 is provided with a plurality of first slits or first openings 318; the grading wheel 313 is a cylindrical structure, and the cylindrical wall of the grading wheel 313 is provided with a plurality of second slits or second openings, and the width of the second slits or second openings 317 widens from the inner side of the cylindrical wall to the outer side. The bottom of the grading wheel 313 has a discharging port.

[0085] The grading mesh plate 312 is mounted on the outside of the grading wheel 313 and is coaxial (concentric) with the first rotating shaft 308. The grading wheel 313 is fixedly connected to the second rotating shaft 319. The mesh plate top cover 320 of the grading mesh plate 312 is fixedly connected to the first rotating shaft 308, and the grading mesh plate 312 thus constitutes the rotating shaft of the crushing section (i.e., the lower section of the first rotating shaft), and the stirring rods 310 are evenly distributed on the outer wall of the grading mesh plate 312 cylinder.

[0086] The width of the first slit or the diameter of the first opening 318 is smaller than the diameter of the grinding ball 311. The ball mill separation device is preferably a cylindrical barrel structure.

[0087] The liquid inlet 303 and the material inlet 301 are located at the top or upper wall of the cylinder of the ball mill separation equipment, and the material distributor 306 is located inside the cylinder. The material inlet 301 is connected to the inlet of the material distributor 306 through a pipeline.

[0088] Preferably, the ball mill separation device further comprises a spiral piece 309, which is located above the crushing section C and fixed on the first rotating shaft 308. The spiral piece 309 selects a conventional structure in the art. For example, the outer diameter of the spiral piece 309 gradually increases from top to bottom, and the outer diameter of the largest spiral piece 309 is half of the inner diameter of the cylinder of the ball mill separation device. The area where the spiral piece 309 is located constitutes a spiral section B, which is located between the feeding section A and the crushing section C, and is located in the middle of the ball mill separation device.

[0089] A motor 305 is arranged outside the top of the cylinder of the quenching and crushing tower 300, and the motor 305 is fixedly connected to the first rotating shaft 308. The first rotating shaft 308 passes through the feeding section A, the spiral section B and the crushing section C. The spiral pieces 309 and the stirring rods 310 are evenly distributed on the first rotating shaft 308 and are fixedly connected to the first rotating shaft 308; the crushing balls 311 are bulked in the crushing section C. The grading discharging module is located at the axis center of the crushing section C.

[0090] There is a gap between the lower edge of the grading mesh plate 312 and the bottom plate of the equipment. The height of the gap should be smaller than the diameter of the crushing ball 311 , and is generally 0.5 to 0.8 times the diameter of the crushing ball 311 .

[0091] The width of the second slit or the diameter of the second opening 317 on the wall of the grading wheel 313 widens from the inside to the outside (i.e., from the center of the circle to the circumference), and the width of the inner slit or the inner opening is generally 0.2 to 0.9 times the width of the outer slit or the outer opening. The width of the inner slit or the opening diameter is generally 2 mm to 15 mm. A sealing cover E is provided at the top of the grading wheel 313, and the sealing cover E is used to prevent the material from entering the grading wheel 313 from the top of the grading wheel. A discharge port 316 is provided at the bottom of the grading wheel 313, and the discharge port 316 is also used as a second rotating shaft 319. The second rotating shaft 319 is connected to the grading motor 321 through the rotating belt 307. The grading mesh plate 312 and the grading wheel 313 can rotate under the drive of the first rotating shaft 308 and the second rotating shaft 319, respectively.

[0092] In the grading mesh plate 312, the width of the first slit or the diameter of the first opening provided on the wall of the grading mesh plate 312 is generally 0.5 to 0.8 times the diameter of the crushing ball 311. The first slit or the first opening provided on the wall of the grading mesh plate 313 is used as a channel for the crushed slurry.

[0093] A rotary quick connector 315 is provided at the lower end of the discharge port 316 of the grading wheel 313, and the other end of the rotary quick connector 315 is connected to the discharge pipe 314. The second rotating shaft 319 penetrates the bottom plate of the equipment and is connected to the grading motor 321 through the rotating belt 307.

[0094] The grading mesh plate 312 is used to isolate the crushing balls 311 to prevent them from entering the grading discharge module, and the grading wheel 313 is used to separate the material powder that meets the particle size requirements.

[0095] like Figure 6-8 As shown, the integrated filtering, washing and drying equipment comprises:

[0096] The filter sleeve 430 is arranged horizontally, and includes an outer sleeve 431 and an inner sleeve 433; the outer sleeve 431 is sleeved outside the inner sleeve 433, and an inner sleeve jacket 435 is arranged in the annular space formed by the outer sleeve 431 and the inner sleeve 433, and the inner sleeve jacket 435 is used to heat the material in the inner sleeve 433; a filter screen 434 is arranged on the inner sleeve wall opposite to the inner sleeve jacket 435, and a filtrate outlet 432 is arranged on the outer sleeve wall corresponding to the filter screen 434;

[0097] The material inlet and outlet cylinder 440 is horizontally arranged and communicated with the filter sleeve 430; the material inlet and outlet cylinder 440 includes a material inlet 441 at the top, a material outlet 444 at the bottom, and a material inlet and outlet cylinder jacket 442;

[0098] The rotating jacket shaft 412 can rotate in the filter sleeve 430; the rotating jacket shaft 412 is composed of an outer shaft tube 413 and an inner shaft tube 414: the inner shaft tube 414 is provided with an shaft heating medium inlet 415, and the outer shaft tube 413 is provided with an shaft heating medium outlet 416; a plurality of distribution branches 418 are provided on the circumferential outer wall of the inner shaft tube 414, and a plurality of stirring paddles 417 are provided on the circumferential outer wall of the outer shaft tube 413, and the plurality of distribution branches 418 are respectively provided corresponding to the plurality of stirring paddles 417, and the outlets of the distribution branches 418 are located in the corresponding internal spaces of the stirring paddles 417.

[0099] An end face flange cover 420 is provided on the end face of the filter sleeve 430. A filtrate outlet 432 is provided at the bottom of the outer cylinder 431, and a filter screen 434 is provided at the bottom of the inner cylinder 433. A vacuum gas outlet 438 is also provided on the side of the outer cylinder 431. Preferably, the arc width of the filter screen 434 is 0.5 to 1.0 times the arc width of the inner cylinder jacket 435. The heat medium inlet 436 and the heat medium outlet 437 of the inner cylinder jacket are both provided on the side of the inner cylinder 433 and pass through the end face flange cover 420.

[0100] The material inlet and outlet tube 440 is a cylindrical jacket structure, which has a diameter equivalent to that of the filter sleeve 430. The heating medium inlet 443 and the heating medium outlet 445 of the material inlet and outlet tube jacket 442 are both arranged at the bottom of the material inlet and outlet tube 440.

[0101] The shaft inner cylinder 414 and the shaft outer cylinder 413 are coaxial central inner and outer sleeves, the shaft heating medium inlet 415 is arranged on the outer wall of the shaft inner cylinder 414, and the shaft heating medium outlet 416 is arranged on the outer wall of the shaft outer cylinder 413. The stirring paddle 417 on the outer wall of the shaft outer cylinder 413 and the distribution branch pipe 418 on the outer wall of the shaft inner cylinder 414 are both located in a closed space formed by the end face flange cover 420, the filter sleeve 430, and the material inlet and outlet cylinder 440.

[0102] The device of the present invention further includes a motor 411, which is used to drive the rotating jacket shaft 412 to rotate. The motor 411 is located at one end of the rotating jacket shaft 412, and the shaft heating medium inlet 415 and the shaft heating medium outlet 416 are located at the other end of the rotating jacket shaft 412. The motor 411 and the shaft heating medium inlet 415 and the shaft heating medium outlet 416 are all located outside the closed space formed by the end face flange cover 420, the filter sleeve 430, and the material inlet and outlet cylinder 440.

[0103] The rotating jacket shaft 412 passes through the end face flange cover 420, the filter sleeve 430 and the material inlet and outlet cylinder 440. The filter sleeve 430 and the material inlet and outlet cylinder 440 are fixedly connected by a flange. The two ends of the filtering, washing and drying device composed of the filter sleeve 430 and the material inlet and outlet cylinder 440 are fixedly sealed by the end face flange cover 420. The filtering, washing and drying device is composed of at least one filter sleeve and at least one material inlet and outlet cylinder 440.

[0104] The two ends of the shaft outer cylinder 413 are connected to the end face flange cover 420 through a sealing member, which can be a mechanical seal, a gas seal or a packing seal. The rotating shaft is driven by the motor 411 to drive the stirring paddle 417 to rotate, and the rotating jacket shaft 412 is used to flow the heating medium to heat the stirring material.

[0105] The filter sleeve is used for filtering, washing and drying integrated equipment, solid-liquid separation and heating. The heating medium can be steam, heat transfer oil or heat medium water.

[0106] Example 2

[0107] This embodiment describes in detail the wet production method of insoluble sulfur of the present invention in conjunction with the accompanying drawings. The method includes the following contents:

[0108] 100-sulfur feed pipeline, 200-polymerization kettle, 300-quenching crushing tower, 400-drying and maturing tank, 500-three-in-one machine, 600-oil-filled kettle, 1-solvent delivery pipe, 2-extractant feed pipe, 3-filtrate discharge pipe, 4-product, 5-delivery solvent feed port, 6-extractant feed port, 7-filtrate outlet; (1) 120℃~130℃ sulfur enters the polymerization kettle 200 through the feed pipe 100, and the sulfur is heated in the polymerization kettle 200 to 250℃~300℃ to obtain high-temperature sulfur. The high-temperature sulfur is kept at a constant temperature of 250℃~300℃ in the polymerization kettle for 1h~2h to obtain the first logistics;

[0109] (2) The first stream enters the quenching and crushing tower 300, where it is quenched by quenching water and crushed in the liquid phase to obtain a slurry-like second stream with a particle size of 0.5 mm to 2 mm;

[0110] (3) The second stream enters the drying and aging tank 400 and is first filtered to separate the quenching water, and then the crude insoluble sulfur is dried by hot air or vacuum. When the water content of the crude insoluble sulfur is less than 1wt%, the crude insoluble sulfur is aged. After the aging, a transport solvent is added to the drying and aging tank 400 to fully mix the solvent with the aged crude insoluble sulfur to obtain a slurry-like third stream.

[0111] (4) The third stream enters the three-in-one machine 500 for filtration, washing, extraction, and drying. After the third stream is filtered, an extractant is added to the three-in-one machine. After the third stream is extracted 2 to 4 times, soluble sulfur is separated, and insoluble sulfur is left in the three-in-one machine. After extraction, the insoluble sulfur is dried to obtain a fourth stream, and the moisture content of the fourth stream is less than 0.5 wt%;

[0112] (5) The fourth logistics enters the oil-filled kettle 600 for further crushing to obtain insoluble sulfur, and after crushing, filling oil is added to obtain a high-performance insoluble sulfur oil-filled product.

[0113] The invention provides a full-process wet production method for insoluble sulfur, and the production process has the characteristics of safety, reliability, simple operation, etc.

Claims

1. A wet production system for insoluble sulfur, characterized in that: It comprises a polymerization kettle, a quenching and crushing tower, a drying and maturing tank, a filtering, washing and drying integrated device and an oil-filled kettle and corresponding connecting pipelines; the feed port of the polymerization kettle is connected to the sulfur feed pipeline, and the discharge port of the polymerization kettle is connected to the feed port of the quenching and crushing tower; the discharge port of the quenching and crushing tower is connected to the feed port of the drying and maturing tank, the discharge port of the drying and maturing tank is connected to the feed port of the filtering, washing and drying integrated device, the discharge port of the filtering, washing and drying integrated device is connected to the feed port of the oil-filled kettle, and the discharge port of the oil-filled kettle is connected to the insoluble sulfur product pipeline; The quenching and crushing tower is a continuous wet ball mill separation device; the continuous wet ball mill separation device comprises a cylinder, the inside of the cylinder comprises a feeding section and a crushing section from top to bottom, and a first rotating shaft is arranged at the center of the cylinder; The feed section is located at the upper part of the ball mill separation equipment, and is provided with a liquid inlet, a material inlet and a material distributor; The crushing section is located at the lower part of the ball mill separation equipment, a stirring rod and a crushing ball are arranged in the crushing section, and a graded discharge module is arranged at the bottom of the crushing section; The grading discharging module comprises a grading mesh plate and a grading wheel; the grading mesh plate is a cylindrical structure, and the mesh plate top cover at the upper end thereof is fixedly connected to the first rotating shaft; the cylindrical wall of the grading mesh plate is provided with a plurality of first slits or first openings; the grading wheel is a cylindrical structure, and the cylindrical wall of the grading wheel is provided with a plurality of second slits or second openings, and the width of the second slits or second openings widens from the inner side of the cylindrical wall to the outer side; the bottom of the grading wheel has a discharging port; The grading mesh plates are sleeved outside the grading wheel and are coaxial with the first rotating shaft; the grading wheel is fixedly connected to the second rotating shaft; and the stirring rods are evenly distributed on the outer wall of the grading mesh plate cylinder.

2. The production system according to claim 1, characterized in that: The drying and maturing tank is provided with a solvent delivery feed port, and the solvent delivery feed port is connected with the solvent delivery pipe.

3. The production system according to claim 1, characterized in that: The filtering, washing and drying integrated equipment is provided with an extractant feed port and a filtrate outlet, the extractant feed port is connected with the extractant feed pipe, and the filtrate outlet is connected with the filtrate discharge pipe.

4. The production system according to claim 1, characterized in that: The polymerization kettle is used to heat ordinary sulfur to 250° C. to 300° C. and maintain the temperature for 1 h to 2 h.

5. The production system according to claim 1, characterized in that: The first slit width or the first opening diameter is smaller than the diameter of the crushing ball.

6. The production system according to claim 1, characterized in that: The liquid inlet and the material inlet are located at the top or upper wall of the cylinder of the ball mill separation equipment, and the material distributor is located inside the cylinder.

7. The production system according to claim 1, characterized in that: The ball mill separation device also includes a spiral sheet, which is located above the crushing section and fixed on the first rotating shaft.

8. The production system according to claim 7, characterized in that: The outer diameter of the spiral sheet increases gradually from top to bottom.

9. The production system according to claim 8, characterized in that: The outer diameter of the largest spiral blade is half of the inner diameter of the ball mill separation equipment cylinder.

10. The production system according to claim 1, characterized in that: A motor is arranged outside the top of the quenching and crushing tower body, and the motor is fixedly connected to the first rotating shaft; the first rotating shaft runs through the feeding section, the spiral section and the crushing section; the spiral sheets and the stirring rods are evenly distributed on the first rotating shaft and fixedly connected to the first rotating shaft; the crushing balls are bulked in the crushing section.

11. The production system according to claim 1, characterized in that: There is a gap between the lower edge of the grading mesh plate and the bottom plate of the equipment, and the height of the gap is smaller than the diameter of the crushing ball.

12. The production system according to claim 1, characterized in that: The second slit width or the second opening diameter widens from the inside to the outside.

13. The production system according to claim 12, characterized in that: The inner width of the second slit is 0.2 to 0.9 times the outer width, and the inner opening width of the second opening is 0.2 to 0.9 times the outer opening width.

14. The production system according to claim 1, characterized in that: In the grading screen plate, the width of the first slit or the diameter of the first opening arranged on the wall of the grading screen plate is 0.5 to 0.8 times the diameter of the crushing ball.

15. The production system according to claim 1, characterized in that: A rotary quick connector is arranged at the lower end of the discharge port of the grading wheel, and the other end of the rotary quick connector is communicated with the discharge pipe.

16. The production system according to claim 1, characterized in that: The drying and maturation tank is used to filter, dry, mature and store the slurry transported from the quenching and crushing tower to obtain a crude insoluble sulfur product; at the same time, a transport solvent is added into the drying and maturation tank, and the transport solvent is mixed with the crude insoluble sulfur product to obtain a fluidized crude insoluble sulfur solid-liquid mixture.

17. The production system according to claim 1, characterized in that: The integrated 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; The material inlet and outlet cylinder is horizontally arranged and communicated with the filter sleeve; the material inlet and outlet cylinder comprises a material inlet at the top, a material outlet at the bottom, and a material inlet and outlet jacket; 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.

18. The production system according to claim 17, characterized in that The filter sleeve and the material inlet and outlet cylinder are fixedly connected via a flange, and both ends of the filtering, washing and drying device composed of the filter sleeve and the material inlet and outlet cylinder are fixedly sealed by end face flange covers.

19. The production system according to claim 17, characterized in that: The filter screen is located at the bottom of the inner cylinder.

20. The production system according to claim 17, characterized in that: A vacuum gas outlet is provided on the side of the outer cylinder.

21. The production system according to claim 17, characterized in that: The arc width of the filter screen is 0.5 to 1.0 times the arc width of the inner tube jacket.

22. The production system according to claim 17, characterized in that: The heat medium inlet 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.

23. The production system according to claim 17, characterized in that: 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.

24. The production system according to claim 17, characterized in that: Also included is a motor, which is used to drive the rotating sleeve shaft to rotate.

25. The production system according to claim 17, characterized in that: The filtering, washing and drying equipment is composed of at least one filtering sleeve and at least one material inlet and outlet cylinder.

26. The production system according to claim 17, characterized in that: The outer wall of the stirring paddle is evenly distributed with fins.

27. A method for producing high-performance insoluble sulfur in a wet process, wherein the insoluble sulfur wet process production system according to any one of claims 1 to 26 is used.

28. The production method according to claim 27, characterized in that It includes the following: (1) Sulfur at 120°C to 130°C enters the polymerization kettle through a feed pipe, and is heated in the polymerization kettle to 250°C to 300°C to obtain high-temperature sulfur. The high-temperature sulfur is kept at a constant temperature of 250°C to 300°C in the polymerization kettle to obtain the first logistics; (2) The first stream enters a quenching and crushing tower, where it is quenched by quenching water and crushed in the liquid phase to obtain a fluidized second stream with a particle size of 0.5 mm to 2 mm; (3) The second stream enters the drying and aging tank and is first filtered to separate the quenching water, and then the crude insoluble sulfur is dried by hot air or vacuum. When the moisture content of the crude insoluble sulfur is less than 1wt%, the crude insoluble sulfur is aged. After the aging, a transport solvent is added to the drying and aging tank to fully mix the solvent with the aged crude insoluble sulfur to obtain a fluidized third stream; (4) The third logistics enters the integrated filtering, washing and drying equipment for filtration, washing, extraction and drying. After the third logistics is filtered, an extractant is added to the integrated filtering, washing and drying equipment. After 2 to 4 extractions, the soluble sulfur is separated, and the insoluble sulfur is left in the integrated filtering, washing and drying equipment. After extraction, the insoluble sulfur is dried to obtain a fourth stream, and the moisture content of the fourth stream is less than 0.5wt%; (5) The fourth logistics enters the oil-filled kettle for further crushing to obtain insoluble sulfur, and after crushing, filler oil is added to obtain a high-performance insoluble sulfur oil-filled product after oil filling.

29. The production method according to claim 28, characterized in that The aging time of step (3) is 24h~50h, and the aging temperature is 50℃~70℃.

30. The production method according to claim 28, characterized in that The constant temperature time in step (1) is 1h~2h.

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