A suspended bed hydrogenation sulfur liquefaction sulfur injection device and a method of using the same

Abstract

The present application belongs to the field of coal chemical industry, and relates to a kind of suspended bed hydrogenation sulfur liquefaction sulfur injection device and its use method.The device comprises a feed hopper, the feed hopper is connected with a crushing bin inlet, a circular screen cylinder is arranged inside the crushing bin, and spherical balls are arranged in the circular screen cylinder, a first outlet is arranged on the top of the crushing bin, and a second outlet is arranged on the bottom of the crushing bin, the first outlet is connected with a dust filter screen, the dust filter screen is connected with a dust collection fan, the second outlet is connected with a feed end of a screw conveyor, a discharge end of the screw conveyor is connected with a jacketed sulfur melting pool, a liquid sulfur outlet, a first steam inlet and a second steam inlet symmetrically distributed are arranged on the side wall of the jacketed sulfur melting pool, a steam condensate outlet is arranged on the bottom of the jacketed sulfur melting pool, a gas outlet is arranged on the top of the jacketed sulfur melting pool, and the gas outlet is connected with a vent filter screen.The present application solves the problems of uneven heating of sulfur and solidification and deposition of liquid sulfur in the prior art.

Description

Technical Field

[0001] This invention belongs to the field of coal chemical industry and relates to a suspended bed hydrogenated sulfur liquefaction and sulfur injection device and its usage method. Background Technology

[0002] In recent years, clean coal processing technologies have developed rapidly, and suspended bed hydrogenation catalysts have become a research hotspot. The catalyst is one of the core elements of the suspended bed hydrogenation process; it only exhibits good activity when in a sulfidated state. Therefore, sulfidation treatment of the catalyst is necessary. Generally, industrial plants choose CS2 or DMDS as sulfiding agents, employing wet or dry sulfidation methods to achieve high catalyst activity. However, CS2 and DMDS are highly toxic and relatively expensive. Through long-term research and improvement, sulfur has been selected as the sulfiding agent. Sulfur powder is mixed with catalyst slurry and transported to the reaction system for catalyst sulfidation.

[0003] In the suspended bed hydrogenation process, the initial method of manually adding solid sulfur suffered from significant mixing unevenness. Solid sulfur powder was difficult to disperse fully in the oil slurry system, leading to inconsistent sulfidation of the catalyst and severely impacting its catalytic activity. Furthermore, manual operation was not only labor-intensive but also posed safety hazards under the high-temperature and high-pressure process environment. While the subsequent improved molten sulfur injection technology improved mixing uniformity to some extent, the large particle size variation and hygroscopic nature of industrial sulfur feedstock often resulted in uneven heating during the melting process. Large pieces of sulfur, due to their low thermal conductivity, often failed to melt completely. Unmelted particles gradually deposited in the low-flow-rate areas of the pipeline during transport, eventually causing blockages and severely affecting the continuity of the unit's operation. In addition, insufficient sulfur melting also led to incomplete sulfidation, preventing the sufficient formation of catalyst active sites and ultimately resulting in unstable product quality and significant fluctuations in impurity content in the product. Summary of the Invention

[0004] To address the problems of uneven heating of sulfur and solidification and deposition of liquid sulfur in existing technologies, this invention provides a suspended bed hydrogenated sulfur liquefaction and injection device and its usage method.

[0005] To achieve the above objectives, the present invention employs the following technical solution: In a first aspect, the present invention provides a suspended bed hydrogenated sulfur liquefaction and sulfur injection device, comprising a feed hopper; the feed hopper is connected to the inlet of a crushing silo; a circular screen is provided inside the crushing silo, and spherical balls are provided inside the circular screen; a first outlet is provided at the top of the crushing silo, and a second outlet is provided at the bottom; the first outlet is connected to a dust filter; the dust filter is connected to a dust collection fan; the second outlet is connected to the feed end of a screw conveyor; the discharge end of the screw conveyor is connected to a jacketed sulfur melting pool; a liquid sulfur outlet and a symmetrically distributed first steam inlet and second steam inlet are provided on the side wall of the jacketed sulfur melting pool, a steam condensate outlet is provided at the bottom, and a gas outlet is provided at the top; the gas outlet is connected to a venting filter.

[0006] Preferably, a nitrogen inlet is provided on the side wall of the dust filter; the nitrogen inlet is connected to a nitrogen solenoid valve.

[0007] Preferably, an air release solenoid valve is provided between the dust filter and the dust collection fan.

[0008] Preferably, the first steam inlet is connected to the first steam valve; the second steam inlet is connected to the second steam valve.

[0009] Preferably, it includes a remote level gauge, the detection end of which is located inside the jacketed sulfur melting pool.

[0010] Preferably, it includes a remote thermometer, the detection end of which is located inside the jacketed sulfur melting pool.

[0011] Preferably, the steam condensate outlet and the steam condensate drain valve are connected.

[0012] Preferably, a stirrer is provided inside the jacketed sulfur melting pool.

[0013] Preferably, the liquid sulfur outlet is connected to the liquid sulfur pump.

[0014] Secondly, the present invention provides a method for using a suspended bed hydrogenated sulfur liquefaction and sulfur injection device, comprising the following steps: Sulfur enters the crushing hopper through the feed hopper and is crushed into sulfur powder by spherical rollers inside the circular screen. The dust generated during the crushing process is filtered through a dust filter, and the filtered gas is discharged through a dust collection fan. The sulfur powder is then screened through the circular screen and conveyed into the jacketed sulfur melting pool by a screw conveyor. Steam enters the jacketed sulfur melting pool through the first steam inlet and the second steam inlet to uniformly heat the sulfur powder. The generated steam condensate is discharged through the steam condensate outlet, and the gas generated in the jacketed sulfur melting pool is filtered through a venting filter and then discharged.

[0015] Compared with the prior art, the present invention has the following beneficial effects: By rotating the circular sieve cylinder, the spherical balls inside crush the damp sulfur, so that the sulfur before entering the molten sulfur pool is in powder form, increasing the heating area of ​​the sulfur; at the same time, by changing the heating method and increasing the heating of the jacket cavity, steam is introduced into the jacket cavity to improve the heating efficiency and allow the sulfur to be fully heated and liquefied.

[0016] Furthermore, the present invention includes a dust filter and a dust collection fan installed on the top of the crushing hopper to prevent sulfur dust from spreading in the air and causing environmental pollution.

[0017] Furthermore, under the action of the stirrer, the unmelted sulfur powder and liquid sulfur are fully mixed and liquefied by heat. The generated gas is filtered and then enters the venting system to prevent harmful gases from polluting the environment. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the structure of a suspended bed hydrogenated sulfur liquefaction and sulfur injection device according to the present invention; Figure 2 This is a cross-sectional view of the circular sieve cylinder of the present invention.

[0020] The components include: 1. Feed hopper; 2. Crushing bin; 3. Nitrogen solenoid valve; 4. Air release solenoid valve; 5. Dust collector fan motor; 6. Jacketed sulfur melting pool; 7. Dust collector fan; 8. Dust filter screen; 9. Circular screen cylinder; 10. Screw conveyor motor; 11. Screw conveyor; 12. Agitator motor; 13. Air release filter screen; 14. Remote level gauge; 15. First steam valve; 16. Remote thermometer; 17. Agitator; 18. Second steam valve; 19. Jacketed liquid sulfur conveying pipe; 20. Steam condensate drain valve; 21. Liquid sulfur pump motor; 22. Liquid sulfur pump; 23. Screen cylinder motor. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0022] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the invention without inventive effort are within the scope of protection of the invention.

[0023] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0024] In the description of the embodiments of the present invention, it should be noted that if terms such as "upper," "lower," "horizontal," or "inner" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of the invention is in use, they are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention. Furthermore, terms such as "first" and "second" are only used to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0025] Furthermore, the use of the term "horizontal" does not imply that the component must be absolutely horizontal, but rather that it can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal than "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0026] In the description of the embodiments of the present invention, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in the present invention according to the specific circumstances.

[0027] The present invention will now be described in further detail with reference to the accompanying drawings: The first objective of this invention is to provide a suspended bed hydrogenated sulfur liquefaction and sulfur injection device, such as... Figure 1 and Figure 2As shown, it includes a feed hopper 1, which is connected to the inlet of a crushing silo 2; the crushing silo 2 is equipped with a circular screen cylinder 9, and the circular screen cylinder 9 is equipped with spherical balls; the crushing silo 2 is equipped with a first outlet at the top and a second outlet at the bottom; the first outlet is connected to a dust filter 8; the dust filter 8 is connected to a dust collection fan 7; the second outlet is connected to the feed end of a screw conveyor 11; the discharge end of the screw conveyor 11 is connected to a jacketed sulfur melting pool 6; the jacketed sulfur melting pool 6 is equipped with a liquid sulfur outlet and symmetrically distributed first and second steam inlets on its side wall, a steam condensate outlet at the bottom, and a gas outlet at the top; the gas outlet is connected to a venting filter 13.

[0028] This invention uses a feed hopper 1 as the initial inlet for sulfur, connected to the inlet of the downstream crushing silo 2, to ensure directional material transport. The crushing silo 2 is equipped with a circular screen cylinder 9. Spherical balls arranged inside the screen cylinder 9 crush the lumpy sulfur into uniform powder through collision and friction as the cylinder rotates. Simultaneously, the mesh structure of the screen cylinder 9 classifies and screens the particles by size, with the fine powder falling to the bottom of the crushing silo 2. The circular screen cylinder 9 is powered by a screen cylinder motor 23, and its rotation speed can be controlled by a frequency converter, adjusting the speed according to the crushing situation. The first outlet at the top of the crushing silo 2 is connected to a dust filter 8, which, together with a dust collector fan 7, actively sucks up suspended sulfur dust, preventing it from escaping into the atmosphere. The second outlet at the bottom of the crushing silo 2 is connected to the feed end of a screw conveyor 11, which continuously and stably feeds the sulfur powder into the jacketed sulfur melting pool 6 through the closed pushing action of the screw blades. The screw conveyor 11 is powered by a screw conveyor motor 10. The jacketed sulfur melting pool 6 adopts a steam jacket structure. The first and second steam inlets symmetrically distributed on its sidewalls ensure uniform heat penetration, allowing the sulfur to fully melt into a liquid state. The bottom steam condensate outlet promptly discharges condensate to maintain heating efficiency, and the top gas outlet is purified by the vent filter 13 before being discharged into the vent main pipe to prevent sulfur-containing gas from polluting the environment. Finally, the molten liquid sulfur flows through the liquid sulfur outlet on the sidewall to the jacketed liquid sulfur conveying pipe 19, and is pumped to the catalyst oil slurry storage tank by the liquid sulfur pump 22, which is powered by the liquid sulfur pump motor 21.

[0029] For example, there are multiple spherical balls with varying diameters. This invention employs a multi-diameter spherical ball combination design, which significantly improves the processing quality and efficiency of the sulfur crushing process through differentiated mechanical action. Larger diameter balls, due to their superior mass, generate a powerful impact, effectively breaking down lumps or agglomerates in the sulfur raw material, fundamentally solving the problem of large particles clogging the screen cylinder. Meanwhile, smaller diameter balls perform fine grinding of the material through high-frequency rolling friction, resulting in a more uniform fineness distribution of sulfur particles, allowing the subsequent melting process to obtain raw materials with a more optimized specific surface area.

[0030] A nitrogen inlet is provided on the side wall of the dust filter 8, and the nitrogen inlet is connected to the nitrogen solenoid valve 3. When fine dust generated during the sulfur crushing process is adsorbed onto the surface of the dust filter 8 by the airflow, low-pressure nitrogen is injected into the dust filter 8 in a pulsed manner through the intermittent opening of the nitrogen solenoid valve 3, forming a reverse airflow impact that effectively removes the adhering dust and prevents the pores of the dust filter 8 from clogging. At the same time, the inert properties of nitrogen can isolate oxygen, avoiding the risk of combustion and explosion of sulfur dust due to static electricity or high temperature during the filtration process, ensuring the safe operation of the system. This design maintains the continuous filtration efficiency of the dust filter 8 and achieves manual cleaning-free operation through automated control, further improving the environmental friendliness and operational stability of the device.

[0031] An air release solenoid valve 4 is installed between the dust filter 8 and the dust collection fan 7, and the dust collection fan 7 is powered by the dust collection fan motor 5. Through the intelligent opening and closing regulation of the air release solenoid valve 4, precise control of the dust airflow is achieved during the continuous operation of the dust collection fan 7. When the dust filter 8 needs nitrogen backflushing for cleaning, the air release solenoid valve 4 can quickly cut off the connection between the dust filter 8 and the dust collection fan 7 to prevent low-pressure nitrogen from flowing back into the dust collection fan 7 and causing disturbance. Under normal filtration conditions, the air release solenoid valve 4 remains unobstructed, ensuring that the dust-laden gas is efficiently drawn and collected by the dust collection fan 7 after passing through the dust filter 8, and the dust is intercepted inside the dust filter 8, while the air and nitrogen are discharged through the dust collection fan 7. Secondly, when dust accumulates inside the dust filter 8, the nitrogen solenoid valve 3 opens to blow away the dust inside the dust filter 8, causing the dust to fall and detach from the dust filter 8. This prevents the dust filter 8 from clogging due to excessive dust, which could lead to insufficient airflow at the inlet of the dust collector fan 7 and cause the dust collector fan 7 to malfunction.

[0032] The first steam inlet is connected to the first steam valve 15; the second steam inlet is connected to the second steam valve 18. By precisely adjusting the flow rate and pressure of the corresponding steam inlets using the first steam valve 15 and the second steam valve 18, omnidirectional and balanced heating of the jacketed sulfur melting pool 6 is achieved. The symmetrically distributed steam injection points create a stable heat flow distribution within the jacket cavity, effectively eliminating the temperature gradient problem that is prone to occur in traditional single-sided heating methods, ensuring that sulfur in all parts of the jacketed sulfur melting pool 6 receives a consistent heat supply. The advantage of independent dual-valve control lies in its ability to flexibly adjust the steam supply ratio on both sides according to real-time operating conditions. It can also respond quickly when a local temperature anomaly is detected, eliminating potential overheated or underheated areas by dynamically balancing the steam flow.

[0033] The sulfur injection device of this invention also includes a remote level gauge 14 and a remote thermometer 16, the detection ends of which are both located inside the jacketed molten sulfur pool 6. The remote level gauge 14 monitors the amount of liquid sulfur stored in the molten sulfur pool in real time, providing a precise signal for the start and stop of the liquid sulfur pump 22 outside the liquid sulfur outlet, ensuring that the liquid level is maintained within the optimal operating range and preventing liquid sulfur from overflowing or being pumped out. The remote thermometer 16 continuously monitors the temperature change of the molten system, and through linkage control with the steam valve, realizes closed-loop regulation of the heating system to maintain a stable sulfurization reaction temperature environment.

[0034] The steam condensate outlet is connected to the steam condensate drain valve 20, which can automatically discharge the condensate generated during the steam heating process, thus avoiding uneven heating caused by the accumulation of condensate.

[0035] A stirrer 17 is installed inside the jacketed sulfur melting pool 6, and the stirrer 17 is powered by a stirrer motor 12. The stirrer 17 generates forced convection through mechanical rotation, causing the liquid sulfur in the melting pool to form a uniform flow state, effectively breaking the agglomeration of unmelted sulfur powder, promoting full contact between solid particles and the high-temperature liquid medium, and significantly improving heat transfer efficiency. At the same time, the stirring action prevents local overheating or deposition of liquid sulfur during the heating process, maintains the temperature uniformity of the entire molten system, and avoids the accumulation of residue at the bottom.

[0036] A second objective of this invention is to provide a method for using a suspended bed hydrogenated sulfur liquefaction and injection device, comprising the following steps: Sulfur enters the crushing hopper 2 through the feed hopper 1 and is crushed into sulfur powder by the spherical rollers in the circular screen cylinder 9. The dust generated during the crushing process is filtered by the dust filter screen 8, and the filtered gas is discharged through the dust collection fan 7. The sulfur powder is then screened by the circular screen cylinder 9 and conveyed into the jacketed sulfur melting pool 6 by the screw conveyor 11. Steam enters the jacketed sulfur melting pool 6 through the first steam inlet and the second steam inlet to uniformly heat the sulfur powder. The generated steam condensate is discharged through the steam condensate outlet, and the gas generated in the jacketed sulfur melting pool 6 is discharged after being filtered by the vent filter screen 13.

[0037] The method of this invention achieves efficient and safe conversion of sulfur from solid to liquid through a systematic process. After sulfur is introduced into the crushing bin 2 through the feed hopper 1, the spherical balls in the circular screen cylinder 9 mechanically crush the sulfur. The dust filter 8, together with the dust collection fan 7, captures the sulfur dust raised during the crushing process. After being crushed, the sulfur powder is screened through the circular screen cylinder 9 and then quantitatively transported to the jacketed sulfur melting pool 6 by the screw conveyor 11. The steam introduced through the first steam inlet and the second steam inlet forms a uniform heating environment in the jacketed sulfur melting pool 6. The steam condensate outlet promptly discharges condensate to maintain heat exchange efficiency, and the venting filter 13 purifies the gas generated during the sulfur melting process.

[0038] Example Taking a suspended bed hydrogenation unit in a factory as an example, the sulfurizing agent selected for this unit is industrial sulfur. During operation, the sulfur injection system often experiences uneven heating of sulfur in the molten sulfur pool, resulting in the mixing of liquid sulfur and solid sulfur, which causes the system to be unable to transport or to block the transport pipeline. Liquid sulfur solidifies on the auxiliary instruments in the molten sulfur pool, causing the instruments to malfunction. A large amount of solid sulfur fails to melt and settles at the bottom of the molten sulfur pool.

[0039] Therefore, the factory uses the suspended bed hydrogenated sulfur liquefaction and sulfur injection device of the present invention to prepare the catalyst sulfiding agent. The specific implementation steps are as follows: Before operation, a certain number of circular balls of different diameters are placed into the circular screen cylinder 9. The screen cylinder motor 23 is started and the speed is adjusted to 20% by frequency conversion. The screw conveyor 11 is started, the first steam valve 15 and the second steam valve 18 are opened, and the jacketed sulfur melting pool 6 is preheated for 20 minutes. The steam condensate drain valve 20 is opened to drain the liquid. The temperature is observed by the remote thermometer 16 and is close to 80℃.

[0040] Sulfur is fed into the crushing hopper 2 through the feed hopper 1. The circular screen cylinder 9 rotates under the drive of the screen cylinder motor 23. The frequency of the screen cylinder motor 23 is adjusted to increase the speed. The spherical balls of different diameters inside collide with each other and grind the sulfur, breaking it into fine powder. The sulfur dust generated during the crushing process rises with the airflow and is intercepted by the dust filter 8. The filtered gas is discharged by the dust collection fan 7 to prevent dust from escaping and polluting the environment. Sulfur powder meeting the particle size requirements is screened through a circular sieve cylinder 9 and falls into a screw conveyor 11. It then enters the jacketed sulfur melting pool 6 via the screw conveyor 11. The first steam valve 15 and the second steam valve 18 control the steam flow rate, allowing steam to enter the jacket layer through the first steam inlet and the second steam inlet, uniformly heating the sulfur melting pool and raising the temperature inside the pool to about 130~150℃. By observing the remote liquid level gauge 14, when the liquid level is greater than 30%, the agitator motor 12 is started to stir the liquid sulfur, promoting the mixing of sulfur powder and liquid sulfur and improving the melting efficiency. When the liquid level on the remote liquid level gauge 14 reaches 45%, the liquid sulfur pump motor 21 is started to transport the liquid sulfur to the catalyst oil slurry tank.

[0041] During operation, the nitrogen solenoid valve 3 opens intermittently to purge nitrogen from the dust filter 8, preventing clogging and ensuring filtration efficiency. Steam condensate is automatically discharged through the steam condensate trap 20 to maintain heating efficiency. Sulfur-containing gases generated during sulfur melting are purified by the vent filter 13 before being discharged, preventing the escape of harmful gases.

[0042] This embodiment avoids the above problems by modifying the liquid sulfur injection device, and the sulfur injection system performs well during operation.

[0043] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A suspended bed hydrogenated sulfur liquefaction and sulfur injection device, characterized in that, Includes a feed hopper (1); the feed hopper (1) is connected to the inlet of the crushing silo (2); the crushing silo (2) is equipped with a circular screen cylinder (9) and spherical balls are provided inside the circular screen cylinder (9); the crushing silo (2) is equipped with a first outlet at the top and a second outlet at the bottom; the first outlet is connected to a dust filter (8); the dust filter (8) is connected to a dust collector fan (7); the second outlet is connected to the feed end of a screw conveyor (11); the discharge end of the screw conveyor (11) is connected to a jacketed sulfur melting pool (6); the jacketed sulfur melting pool (6) is equipped with a liquid sulfur outlet and a symmetrically distributed first steam inlet and second steam inlet on its side wall, a steam condensate outlet at the bottom, and a gas outlet at the top; the gas outlet is connected to a venting filter (13). A nitrogen inlet is provided on the side wall of the dust filter (8); the nitrogen inlet is connected to the nitrogen solenoid valve (3); An air release solenoid valve (4) is provided between the dust filter (8) and the dust collection fan (7). The first steam inlet is connected to the first steam valve (15); the second steam inlet is connected to the second steam valve (18); It also includes a remote level gauge (14), the detection end of which is located inside the jacketed sulfur melting pool (6); It also includes a remote thermometer (16), the detection end of which is located inside the jacketed sulfur melting pool (6); The steam condensate outlet and the steam condensate drain valve (20) are connected; A stirrer (17) is installed inside the jacketed sulfur melting pool (6). The liquid sulfur outlet is connected to the liquid sulfur pump (22).

2. The method of using the suspended bed hydrogenated sulfur liquefaction and sulfur injection device according to claim 1, characterized in that, Includes the following steps: Sulfur enters the crushing hopper (2) through the feed hopper (1), and is crushed into sulfur powder by the spherical ball bearings in the circular screen (9). The dust generated during the crushing process is filtered by the dust filter (8), and the filtered gas is discharged through the dust collector (7). The sulfur powder is then screened by the circular screen (9) and transported into the jacketed sulfur melting pool (6) by the screw conveyor (11). Steam enters the jacketed sulfur melting pool (6) through the first steam inlet and the second steam inlet, and heats the sulfur powder evenly. The generated steam condensate is discharged through the steam condensate outlet. The gas generated in the jacketed sulfur melting pool (6) is filtered through the vent filter (13) and then discharged.

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