Apparatus and method for recovering sulfur from hydrogen sulfide by thermal catalytic cracking

Abstract

The application discloses a device and a method for recovering sulfur by hydrogen sulfide thermal catalytic cracking, belongs to the technical field of hydrogen sulfide catalytic cracking, and comprises successively connected gas inlet devices, hollow reaction tubes, condensers and sulfur collecting devices. The hollow reaction tubes are arranged in heating furnaces, heat preservation structures are arranged outside connecting pipelines of the hollow reaction tubes and the condensers, inverted catalyst placing tubes are arranged in the hollow reaction tubes, a plurality of through holes are formed in the bottom of each catalyst placing tube and are communicated with the upper space of the hollow reaction tube, different catalysts are respectively filled in the inside of each catalyst placing tube and the upper space of the hollow reaction tube. The application can realize controllable bed layer height of the catalyst, controllable proportion of the two kinds of catalysts and space separation, effectively recovers the sulfur, avoids the occurrence of sulfur blockage, and simultaneously improves the hydrogen sulfide reaction conversion rate and the total sulfur recovery rate.

Description

Technical Field

[0001] This invention relates to the field of hydrogen sulfide catalytic cracking technology, specifically to an apparatus and method for recovering sulfur through hydrogen sulfide thermocatalytic cracking. Background Technology

[0002] Hydrogen sulfide is a toxic gas that pollutes the environment and is widely present in industries such as oil and gas extraction, petrochemicals, and coal chemicals. Hydrogen sulfide not only harms human health, but also causes corrosion of metals and other materials, environmental damage, ecological pollution, and economic waste. Therefore, it is crucial to treat and utilize hydrogen sulfide in a harmless manner.

[0003] Direct hydrogen sulfide cracking is an ideal technology route for the resource utilization of hydrogen sulfide. It can render hydrogen sulfide harmless, produce elemental sulfur, and generate high-value-added hydrogen, meeting atom economy requirements. It is a promising reserve technology for hydrogen sulfide treatment. Hydrogen sulfide thermocatalytic cracking technology is currently the optimal solution for industrial application due to its simplicity. It uses thermal energy to break the bonds in hydrogen sulfide, adds a catalyst to lower the activation energy of the thermal decomposition reaction, accelerates the chemical reaction rate, and increases the yield of reaction products. Simultaneously, through recycling, it enhances the hydrogen sulfide treatment capacity.

[0004] In the existing technology, the devices for hydrogen sulfide thermocatalytic cracking have the following defects: 1. They lack a structure for recovering sulfur resources, and some sulfur recovery structures are prone to sulfur blockage in the pipeline during the cooling process; 2. The catalyst bed has poor adjustability, making it difficult to accurately measure the amount of catalyst participating in the reaction, and the amount of catalyst is inconvenient to adjust. Summary of the Invention

[0005] This invention aims to address the technical problems of sulfur blockage and poor catalyst bed adjustability in existing hydrogen sulfide thermocatalytic cracking devices during sulfur resource recovery. The purpose is to provide a device and method for recovering sulfur through hydrogen sulfide thermocatalytic cracking, which enables controllable catalyst bed height, controllable ratio of the two catalysts, and spatial separation, effectively avoiding sulfur blockage, while improving the hydrogen sulfide reaction conversion rate and total sulfur recovery rate.

[0006] This invention is achieved through the following technical solution:

[0007] This invention provides an apparatus for recovering sulfur by thermocatalytic cracking of hydrogen sulfide, comprising an air inlet device, a hollow reaction tube, a condenser and a sulfur collection device connected in sequence.

[0008] The hollow reaction tube is located inside the heating furnace. The connecting pipe between the hollow reaction tube and the condenser is equipped with a heat insulation structure. An inverted catalyst placement tube is installed inside the hollow reaction tube. The bottom of the catalyst placement tube has multiple through holes that communicate with the upper space of the hollow reaction tube. Different catalysts are filled inside the catalyst placement tube and in the upper space of the hollow reaction tube.

[0009] As a further technical solution of the present invention, the air intake device includes a hydrogen sulfide storage tank and a mass flow meter. The hydrogen sulfide storage tank is connected to the hollow reaction tube through an air intake pipe, and the mass flow meter is installed on the air intake pipe.

[0010] As a further technical solution of the present invention, the internal cavity of the heating furnace is filled with heat-insulating material, and a silicon carbide heating rod is provided inside the heating furnace.

[0011] As a further technical solution of the present invention, a temperature measuring device is provided inside the hollow reaction tube, the temperature measuring device including a corundum temperature measuring sleeve and a thermocouple disposed inside the corundum temperature measuring sleeve.

[0012] As a further technical solution of the present invention, the heat insulation structure adopts an electric heating jacket.

[0013] As a further technical solution of the present invention, the condenser is a shell-and-tube condenser.

[0014] As a further technical solution of the present invention, the sulfur collection device is connected to an outlet pipe on its side, and the outlet pipe is connected to the tail gas purification pipe and the return pipe through a three-way valve.

[0015] As a further technical solution of the present invention, the exhaust gas purification pipe is connected in sequence to the exhaust gas purification device and the gas chromatography detection device.

[0016] As a further technical solution of the present invention, the reflux pipe is connected to the air inlet of the hollow reaction pipe.

[0017] As a further technical solution of the present invention, the inner wall of the hollow reaction tube is provided with multiple sets of connection holes one, and the side wall of the catalyst placement tube is provided with a set of connection holes two. The two ends of the elastic retaining spring pass through the connection holes one and the connection holes two to achieve fixation.

[0018] This invention also provides a method for recovering sulfur by thermocatalytic cracking of hydrogen sulfide, comprising the following steps:

[0019] S1, Catalyst loading

[0020] Based on the required catalyst bed height and catalyst dosage, the inverted catalyst placement tube is fixed at a suitable height inside the hollow reaction tube. Catalyst A is filled in the upper space of the hollow reaction tube, and catalyst B is filled inside the catalyst placement tube.

[0021] S2, Initiating the reaction

[0022] Start the equipment, power on the heating furnace to raise the temperature, and introduce hydrogen sulfide gas into the hollow reaction tube. The hydrogen sulfide gas passes through catalyst A and catalyst B in sequence to react, and then flows out from the outlet of the hollow reaction tube, passes through the heat preservation structure and enters the condenser to be condensed. Sulfur is recovered in the sulfur collection device.

[0023] S3, Reaction Cycle

[0024] Of the gas flowing out of the sulfur collection device, a portion flows back to the hollow reaction tube for a secondary reaction, while the remaining portion is purified and enters a gas chromatograph to determine the single-stage conversion rate.

[0025] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0026] 1. This invention, by setting an inverted catalyst placement tube inside a hollow reaction tube, allows for adjustment of the height of the catalyst placement tube within the hollow reaction tube as needed. This achieves the technical effects of controllable catalyst bed height, controllable ratio of upper and lower catalysts, and spatial separation, enabling multi-stage reactions. By setting a heat insulation structure outside the connecting pipe between the hollow reaction tube and the condenser, efficient recovery of product sulfur resources can be achieved, and sulfur blockage can be effectively avoided.

[0027] 2. This invention, by setting an inverted catalyst placement tube inside a hollow reaction tube, spatially separates the two catalysts and allows them to react sequentially. This effectively improves the hydrogen sulfide reaction conversion rate and total sulfur recovery rate. Furthermore, the catalyst placement tube can be adjusted as needed, making it more convenient to control the catalyst bed height, catalyst ratio, and dosage. Attached Figure Description

[0028] To more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly described below. It should be understood that the following drawings only show some embodiments of the present invention and should not be considered as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort. In the drawings:

[0029] Figure 1 This is a schematic diagram of the structure of the device of the present invention;

[0030] Figure 2 This is a schematic diagram of the connection structure between the catalyst placement tube and the hollow reaction tube.

[0031] The attached diagram shows the markings and corresponding component names:

[0032] 1-Hydrogen sulfide storage tank, 2-Mass flow meter, 3-Heating furnace, 4-Hollow reaction tube, 401-Connection hole one, 5-Vacuum flange, 6-Temperature measuring device, 7-Catalyst placement tube, 701-Connection hole two, 702-Through hole, 8-Silicon carbide heating rod, 9-Insulation structure, 10-Condenser, 11-Sulfur collection device, 12-Three-way valve, 13-Reflux pipe, 14-Tail gas purification pipe, 15-Tail gas purification device, 16-Gas chromatography detection device, 17-Elastic snap ring. Detailed Implementation

[0033] To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the embodiments and accompanying drawings. The illustrative embodiments and descriptions of the present invention are only used to explain the present invention and are not intended to limit the present invention.

[0034] In the following description, numerous specific details are set forth in order to provide a thorough understanding of the invention. However, it will be apparent to those skilled in the art that these specific details are not necessary to practice the invention. In other embodiments, well-known structures, circuits, materials, or methods have not been specifically described in order to avoid obscuring the invention.

[0035] Example 1

[0036] This embodiment provides an apparatus for recovering sulfur by thermocatalytic cracking of hydrogen sulfide, comprising an air inlet device, a hollow reaction tube 4, a condenser 10 and a sulfur collection device 11 connected in sequence;

[0037] The hollow reaction tube 4 is located inside the heating furnace 3. The connecting pipe between the hollow reaction tube 4 and the condenser 10 is provided with a heat insulation structure 9. An inverted catalyst placement tube 7 is provided inside the hollow reaction tube 4. The bottom of the catalyst placement tube 7 has multiple through holes 702 that communicate with the upper space of the hollow reaction tube 4. Different catalysts are filled inside the catalyst placement tube 7 and the upper space of the hollow reaction tube 4, respectively.

[0038] This invention achieves the technical effects of controllable catalyst bed height, controllable ratio of upper and lower catalysts, and spatial separation by setting an inverted catalyst placement tube 7 inside the hollow reaction tube 4, which can adjust the height of the catalyst placement tube 7 inside the hollow reaction tube 4 as needed. By setting a heat insulation structure 9 outside the connecting pipe between the hollow reaction tube 4 and the condenser 10, the efficient recovery of product sulfur resources can be achieved and sulfur blockage can be effectively avoided.

[0039] The gas inlet device includes a hydrogen sulfide storage tank 1 and a mass flow meter 2. The hydrogen sulfide storage tank 1 is connected to the hollow reaction tube 4 through a gas inlet pipe. The mass flow meter 2 is installed on the gas inlet pipe and is made of corrosion-resistant material. It is used to measure the mass flow rate of hydrogen sulfide gas.

[0040] The heating furnace 3 has an internal cavity filled with insulation material and a silicon carbide heating rod 8 inside. Specifically, the heating furnace 3 is a single-stage vertical, open-type insulated reactor, equipped with an electrical control system that can precisely control the heating temperature to 300-1600℃. The internal cavity insulation layer is thicker than 10cm, and has high temperature resistance, good heating stability and temperature uniformity. It can achieve furnace temperature control from RT to 1600℃, with an overshoot temperature of less than 10℃, and has an over-temperature alarm function.

[0041] The hollow reaction tube 4 is equipped with a temperature measuring device 6, which includes a corundum temperature measuring sleeve and a thermocouple installed inside the corundum temperature measuring sleeve. The thermocouple is controlled by a temperature controller, with a temperature control range of room temperature to 1600℃ and a temperature control accuracy of ≤1℃.

[0042] The insulation structure 9 is an electric heating jacket. Since the connection between the hollow reaction tube 4 and the condenser 10 is most prone to sulfur blockage, this invention designs the connecting pipe with an enlarged inner diameter and a shortened length, and sets up an insulation structure 9 for insulation. The pipe length is 1-3cm, the outer diameter is 1-2cm, and the inner diameter is 0.8-1.8cm. The insulation structure 9 of the pipe is a flexible electric heating jacket, which insulates the pipe and controls the temperature of the gas in the pipe, avoids rapid cooling from high temperature, improves the service life of the device, and effectively prevents sulfur from cooling and condensing at this point, thus preventing blockage of the pipe.

[0043] The condenser 10 is a shell-and-tube condenser 10; specifically, the diameter of the shell-and-tube condenser 10 is 8-15cm, the height is 15-20cm, and it contains 6-10 heat exchange tube bundles. The heat exchange tube bundles are connected to the tube sheet, the tube sheet is welded to both ends of the shell, and the shell is equipped with fluid inlet and outlet pipes. The connection between the tube bundles and the tube sheet and the shell is rigid. The condensate flowing outside the heat exchange tube bundles cools the gas inside the tubes. The temperature of the condensate is 10-20℃, so that the sulfur vapor is completely cooled and solidified into sulfur in this part.

[0044] The sulfur collection device 11 has an outlet pipe connected to its side. The outlet pipe is connected to the tail gas purification pipe 14 and the return pipe 13 via a three-way valve 12. The tail gas purification pipe 14 is connected to the tail gas purification device 15 and the gas chromatograph detection device 16 in sequence. The return pipe 13 is connected to the inlet of the hollow reaction tube 4. By setting the three-way valve 12 to control the flow, 1 / 20 to 1 / 10 of the gas enters the detection unit to determine the single-stage conversion rate, and 19 / 20 to 9 / 10 of the gas is circulated to the hollow reaction tube 4 to realize the simultaneous detection of the reaction tail gas and to carry out secondary reaction before returning to the reaction unit, thus promoting the reaction conversion. Specifically, the tail gas purification device 15 is equipped with quartz wool and calcium chloride to dry and purify the tail gas, while avoiding contamination of the detection system by impurities.

[0045] Among them, such as Figure 2 As shown, the inner wall of the hollow reaction tube 4 has multiple sets of connection holes 401, and the side wall of the catalyst placement tube 7 has a set of connection holes 701. The two ends of the elastic retaining spring 17 pass through the connection holes 401 and 701 to fix the hollow reaction tube 4 and the catalyst placement tube 7. It should be understood that the connection hole 401 is a non-through hole to avoid gas leakage, while the connection hole 701 and the through hole 702 are both through holes.

[0046] Specifically, the hollow reaction tube 4 is a corundum reaction tube or a high-temperature quartz reaction tube, sealed by a vacuum flange 5, hollow at both ends, 30cm to 80cm long, with an inner diameter of 1 to 5cm and an outer diameter of 1.5 to 7cm. A connecting hole 401 is formed by drilling holes in the inner wall of the hollow reaction tube 4, with a diameter of 1 to 2mm. The catalyst placement tube 7 is inverted inside the hollow reaction tube 4. The catalyst placement tube 7 is a high-temperature resistant corundum tube, 10cm to 35cm long, with an inner diameter of 0.5 to 4.5cm and an outer diameter of 1 to 5cm. Its outer diameter is adapted to the inner diameter of the hollow reaction tube 4. A through hole 702 is formed at the bottom, with a diameter of 0.1 to 1mm.

[0047] It should be understood that, in order to achieve the separation of the upper and lower catalyst layers by the catalyst placement tube 7, the size of the through hole 702 at the bottom of the catalyst placement tube 7 should be smaller than the size of the upper catalyst layer, so as to ensure that the upper catalyst layer does not enter the interior of the catalyst placement tube 7 and achieve physical separation of the two catalyst layers.

[0048] When it is necessary to adjust the height of the two catalyst beds or the ratio of catalyst dosage, the two ends of the elastic retaining spring 17 are inserted into the connecting holes 701 on the side wall of the catalyst placement tube 7. The catalyst placement tube is moved up and down to the required position. After the height is adjusted and suitable, the two ends of the elastic retaining spring 17 are inserted into the connecting holes 401 on the side wall of the hollow reaction tube 4, thereby fixing the hollow reaction tube 4 to the catalyst placement tube 7. Figure 2 As shown, the connecting holes 401 on the side wall of the hollow reaction tube 4 are arranged in multiple rows, which facilitates the adjustment of the height of the catalyst placement tube 7.

[0049] Example 2

[0050] This embodiment, based on the apparatus of Embodiment 1, provides a method for recovering sulfur through thermocatalytic cracking of hydrogen sulfide, comprising the following steps:

[0051] S1, Catalyst loading

[0052] The hollow reaction tube, sealed with a vacuum flange, is 30cm long, with an inner diameter of 1cm and an outer diameter of 1.5cm. There are 5 pairs of 1mm diameter holes in the inner wall of the hollow reaction tube. The inverted catalyst placement tube is connected internally by elastic spring clips. The two ends of the elastic spring clips are fixed in the first pair of holes from bottom to top in the inner wall of the hollow reaction tube. The bottom of the catalyst placement tube has a 0.1mm diameter hole and a length of 10cm. The inner diameter of the reaction tube is 0.5cm and the outer diameter is 0.9cm.

[0053] The catalysts molybdenum sulfide and alumina are respectively filled in the upper space of the hollow reaction tube and the inside of the catalyst placement tube, with the heights of the two catalyst beds being 8.3 cm and 4.0 cm, respectively.

[0054] S2, Initiating the reaction

[0055] The equipment was started, the heating furnace was powered on and heated to 800℃, and a gas with a concentration of 50% hydrogen sulfide was introduced into the hollow reaction tube at a flow rate of 100 mL / min. The hydrogen sulfide gas passed through molybdenum sulfide and alumina in sequence for 120 min. Then, the gas flowed out from the outlet of the hollow reaction tube, was kept warm by an electric heating jacket (250℃), and entered the condenser for condensation (20℃ condensate). 6.86 g of sulfur was recovered in the sulfur collection device.

[0056] The hollow reaction tube outlet and the condenser connection section have a pipe length of 1cm and an outer diameter of 10mm. The flexible electric heating jacket has a length of 8cm, an internal diameter of 8cm and 1.5cm, and a width of 3cm. The condenser is a shell-and-tube condenser containing 12 heat exchange tube bundles.

[0057] S3, Reaction Cycle

[0058] Gas flows out from the outlet on the side of the sulfur collection device. The flow is controlled and split. 19 / 20 of the gas flows back to the hollow reaction tube for a secondary reaction. 1 / 20 of the gas is purified and enters the gas chromatograph for detection. The single-stage conversion rate is determined to be 50%, and the total sulfur recovery rate of the cyclic reaction is 80%.

[0059] The gas chromatography detection device uses three columns: a 9Ft 1 / 8 2mm MolSieve 13X 45 / 60UM column, a 3Ft 1 / 8 2mm HayeSep Q 80 / 100UM column, and a PLOT Q with PT column, along with a TCD with an EPC detector, to simultaneously detect hydrogen sulfide, hydrogen, organic sulfur, carbon monoxide, and other components in the same chromatogram.

[0060] Example 3

[0061] This embodiment, based on the apparatus of Embodiment 1, provides a method for recovering sulfur through thermocatalytic cracking of hydrogen sulfide, comprising the following steps:

[0062] S1, Catalyst loading

[0063] The hollow reaction tube, sealed with a vacuum flange, is 80cm long, with an inner diameter of 5cm and an outer diameter of 7cm. There are 5 pairs of 1mm diameter holes in the inner wall of the hollow reaction tube. The inverted catalyst placement tube is connected internally by elastic spring clips. The two ends of the elastic spring clips are fixed in the second pair of holes from the bottom to the top of the inner wall of the hollow reaction tube. The bottom of the catalyst placement tube has a 0.1mm diameter hole and is 35cm long. The inner diameter of the reaction tube is 3.5cm and the outer diameter is 4.5cm.

[0064] The catalysts molybdenum sulfide and alumina were respectively filled in the upper space of the hollow reaction tube and the inside of the catalyst placement tube, with the heights of the two catalyst beds being 43.4 cm and 36.6 cm, respectively.

[0065] S2, Initiating the reaction

[0066] The equipment was started, the heating furnace was powered on and heated to 1000℃, and a gas with a concentration of 50% hydrogen sulfide was introduced into the hollow reaction tube at a flow rate of 800 mL / min. The hydrogen sulfide gas passed through molybdenum sulfide and alumina in sequence for 40 min. Then, the gas flowed out from the outlet of the hollow reaction tube, was kept warm by an electric heating jacket (250℃), and entered the condenser for condensation (20℃ condensate). 21.72 g of sulfur was recovered in the sulfur collection device.

[0067] The hollow reaction tube outlet and the condenser connection section are 3cm long and 10mm in outer diameter. The flexible electric heating jacket is 8cm long, with an internal diameter of 8cm and 1.5cm and a width of 3cm. The condenser is a shell-and-tube condenser containing 10 heat exchange tube bundles.

[0068] S3, Reaction Cycle

[0069] Gas flows out from the outlet on the side of the sulfur collection device. The flow is controlled and split. 19 / 20 of the gas flows back to the hollow reaction tube for secondary reaction. 1 / 20 of the gas is purified and enters the gas chromatograph for detection. The single-stage conversion rate is determined to be 58%, and the total sulfur recovery rate of the cyclic reaction is 87%.

[0070] The gas chromatography detection device uses three columns: a 9Ft 1 / 8 2mm MolSieve 13X 45 / 60UM column, a 3Ft 1 / 8 2mm HayeSep Q 80 / 100UM column, and a PLOT Q with PT column, along with a TCD with an EPC detector, to simultaneously detect hydrogen sulfide, hydrogen, organic sulfur, carbon monoxide, and other components in the same chromatogram.

[0071] Example 4

[0072] This embodiment, based on the apparatus of Embodiment 1, provides a method for recovering sulfur through thermocatalytic cracking of hydrogen sulfide, comprising the following steps:

[0073] S1, Catalyst loading

[0074] The hollow reaction tube, sealed with a vacuum flange, is 55cm long, with an inner diameter of 3cm and an outer diameter of 4cm. There are 5 pairs of 1mm diameter holes in the inner wall of the hollow reaction tube. The inverted catalyst placement tube is connected internally by elastic spring clips. The two ends of the elastic spring clips are fixed in the second pair of holes from the bottom to the top of the inner wall of the hollow reaction tube. The bottom of the catalyst placement tube has a 0.1mm diameter hole and a length of 22cm. The inner diameter of the reaction tube is 2cm and the outer diameter is 2.5cm.

[0075] The catalysts molybdenum sulfide and alumina are respectively filled in the upper space of the hollow reaction tube and the inside of the catalyst placement tube, with the heights of the two catalyst beds being 11.3 cm and 9.2 cm, respectively.

[0076] S2, Initiating the reaction

[0077] The equipment was started, the heating furnace was powered on and heated to 1000℃, and a gas with a concentration of 50% hydrogen sulfide was introduced into the hollow reaction tube at a flow rate of 300 mL / min. The hydrogen sulfide gas passed through molybdenum sulfide and alumina in sequence for 40 min. Then, the gas flowed out from the outlet of the hollow reaction tube, was kept warm by an electric heating jacket (250℃), and entered the condenser for condensation (20℃ condensate). 8.13 g of sulfur was recovered in the sulfur collection device.

[0078] The hollow reaction tube outlet and the condenser connection section have a pipe length of 1cm and an outer diameter of 10mm. The flexible electric heating jacket has a length of 8cm, an internal diameter of 8cm and 1.5cm, and a width of 3cm. The condenser is a shell-and-tube condenser, which contains 8 heat exchange tube bundles.

[0079] S3, Reaction Cycle

[0080] Gas flows out from the outlet on the side of the sulfur collection device. The flow is controlled and split. 19 / 20 of the gas flows back to the hollow reaction tube for a secondary reaction. 1 / 20 of the gas is purified and enters the gas chromatograph for detection. The single-stage conversion rate is determined to be 65%, and the total sulfur recovery rate of the cyclic reaction is 95%.

[0081] The gas chromatography detection device uses three columns: a 9Ft 1 / 8 2mm MolSieve 13X 45 / 60UM column, a 3Ft 1 / 8 2mm HayeSep Q 80 / 100UM column, and a PLOT Q with PT column, along with a TCD with an EPC detector, to simultaneously detect hydrogen sulfide, hydrogen, organic sulfur, carbon monoxide, and other components in the same chromatogram.

[0082] The relevant data records for hydrogen sulfide cracking in Examples 2-4 are shown in Table 1.

[0083] Table 1. Data Records Related to Hydrogen Sulfide Cracking in Examples 2-4

[0084]

[0085]

[0086] Comparative Example

[0087] Based on Example 2, this embodiment removes the catalyst placement tube inside the hollow reaction tube and directly fills it with catalyst. The difference is that the catalyst bed height cannot be accurately assessed, and the catalysts are mixed together. The single-stage conversion rate is 45%. Sulfur is recovered and weighed, yielding 5.83g of sulfur. The comparison data between this comparative example and Example 2 are shown in Table 2.

[0088] Table 2. Comparison data between the comparative example and Example 2

[0089] Case Catalyst bed height Catalyst ratio Reaction conversion rate (%) Total sulfur recovery rate (%) Example 2 8.3 cm of molybdenum sulfide + 4.0 cm of aluminum oxide 2∶1 50 80 Comparative Example Molybdenum sulfide and alumina mixed 2∶1 45 68

[0090] A comparison of the data from Example 2 and the comparative example shows that when the catalyst placement tube was removed, both the single-stage conversion rate of hydrogen sulfide and the total sulfur recovery rate of the cyclic reaction decreased. This indicates that the catalyst placement tube spatially separates the two catalysts, allowing them to react sequentially, which effectively improves the hydrogen sulfide reaction conversion rate and the total sulfur recovery rate. Furthermore, the catalyst placement tube can be adjusted as needed, making it more convenient to control the catalyst bed height, catalyst ratio, and dosage.

[0091] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. 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. An apparatus for recovering sulfur by thermal catalytic cracking of hydrogen sulfide, characterized by, The device comprises a gas inlet device, a hollow reaction tube (4), a condenser (10) and a sulfur collection device (11) connected in sequence. The hollow reaction tube (4) is arranged in a heating furnace (3), and an outer connecting pipeline of the hollow reaction tube (4) and the condenser (10) is provided with a heat preservation structure (9); an inverted catalyst placement tube (7) is connected to the hollow reaction tube (4) by an elastic clamp spring (17); a plurality of through holes (702) are formed in the bottom of the catalyst placement tube (7) and are in communication with the upper space of the hollow reaction tube (4); and different catalysts are filled in the catalyst placement tube (7) and the upper space of the hollow reaction tube (4) respectively.

2. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that, The gas inlet device comprises a hydrogen sulfide storage tank (1) and a mass flow meter (2); the hydrogen sulfide storage tank (1) is connected to the hollow reaction tube (4) through a gas inlet pipeline; and the mass flow meter (2) is arranged on the gas inlet pipeline.

3. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that, The internal cavity of the heating furnace (3) is filled with a heat preservation material, and the heating furnace (3) is internally provided with a carbon-silicon heating rod (8).

4. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that, A temperature measuring device (6) is arranged in the hollow reaction tube (4); the temperature measuring device (6) comprises a corundum temperature measuring sleeve and a thermocouple arranged in the corundum temperature measuring sleeve.

5. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that, The heat preservation structure (9) is an electric heating jacket.

6. The device for recovering sulfur by thermal catalytic cleavage of hydrogen sulfide according to claim 1, characterized in that, The condenser (10) is a shell-and-tube condenser.

7. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that, The sulfur collection device (11) is connected with a gas outlet pipeline on the side; the gas outlet pipeline is connected with an exhaust gas purification pipeline (14) and a reflux pipeline (13) through a three-way valve (12).

8. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 7, characterized in that, The exhaust gas purification pipeline (14) is connected with an exhaust gas purification device (15) and a gas chromatography detection device (16) in sequence; and the reflux pipeline (13) is connected with the gas inlet of the hollow reaction tube (4).

9. The device for recovering sulfur by thermal catalytic cleavage of hydrogen sulfide according to claim 1, characterized in that, A plurality of connecting holes one (401) are formed in the inner wall of the hollow reaction tube (4); a group of connecting holes two (701) are arranged through the side wall of the catalyst placement tube (7); and the elastic clamp spring (17) is fixed by penetrating the connecting holes one (401) and the connecting holes two (701) at both ends.

10. A method for recovering sulfur by thermal catalytic cleavage of hydrogen sulfide, characterized by, The device of any one of claims 1-9 is used, comprising the following steps: S1, catalyst filling According to the catalyst bed height and the catalyst dosage requirement, the inverted catalyst placement tube (7) is fixed at a suitable height in the hollow reaction tube (4); catalyst A is filled in the upper space of the hollow reaction tube (4); and catalyst B is filled in the catalyst placement tube (7). S2, starting reaction The device is started; the heating furnace (3) is powered on and heated; hydrogen sulfide gas is introduced into the hollow reaction tube (4); the hydrogen sulfide gas is sequentially reacted with catalyst A and catalyst B; then the hydrogen sulfide gas flows out from the outlet of the hollow reaction tube (4), passes through the heat preservation structure (9) and enters the condenser (10) to be condensed; and sulfur is recovered in the sulfur collection device (11). S3, reaction circulation The gas flowing out from the sulfur collection device (11) is partially returned to the hollow reaction tube (4) to perform secondary reaction; and the other part of the gas is purified and then enters the gas chromatography detection device (16) to determine the single-stage conversion rate.

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