Device and method for recovering sulfur through hydrogen sulfide thermocatalytic cracking

Abstract

The invention discloses a device and method for recovering sulfur through hydrogen sulfide thermocatalytic cracking, and belongs to the technical field of hydrogen sulfide catalytic cracking, the device comprises a gas inlet device, a hollow reaction tube, a condenser and a sulfur collecting device which are connected in sequence, the hollow reaction tube is arranged in a heating furnace, and the condenser is arranged in the heating furnace; a heat preservation structure is arranged outside a connecting pipeline of the hollow reaction pipe and the condenser, an inverted catalyst containing pipe is arranged in the hollow reaction pipe, and a plurality of through holes are formed in the bottom of the catalyst containing pipe and communicated with the upper space of the hollow reaction pipe. The interior of the catalyst placing tube and the upper space of the hollow reaction tube are respectively filled with different catalysts; the bed height of the catalysts can be controlled, the proportion of the two catalysts is controllable, space separation is achieved, sulfur is effectively recycled, the situation of sulfur blockage is avoided, and meanwhile the hydrogen sulfide reaction conversion rate and the total sulfur recovery rate are increased.

Description

Technical Field

[0001] The invention relates to the technical field of hydrogen sulfide catalytic cracking, and in particular to a device and method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide. Background Art

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

[0003] Direct cracking of hydrogen sulfide is an ideal technology route for the resource utilization of hydrogen sulfide. It can make hydrogen sulfide harmless, produce elemental sulfur, and generate high-value-added hydrogen. It is in line with atom economy and is a hydrogen sulfide treatment reserve technology with application prospects. Hydrogen sulfide thermal catalytic cracking technology is the optimal solution for industrial application due to its simple process. It provides energy for hydrogen sulfide bond breaking through thermal energy, adds catalysts to reduce the activation energy of thermal decomposition reaction, accelerates the chemical reaction rate, and improves the yield of reaction products. At the same time, through cyclic reactions, it improves the hydrogen sulfide treatment capacity.

[0004] In the prior art, the devices for thermal catalytic cracking of hydrogen sulfide have the following defects: 1. There is a lack of 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, which makes it difficult to accurately measure the amount of catalyst involved in the reaction and makes it inconvenient to adjust the amount of catalyst. Summary of the invention

[0005] The present invention aims to solve the technical problems that the existing hydrogen sulfide thermal catalytic cracking device is prone to sulfur blockage and the catalyst bed has poor adjustability when recovering sulfur resources. The present invention aims to provide a device and method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide, which can realize controllable catalyst bed height, controllable ratio of two catalysts and spatial separation, effectively avoid sulfur blockage, and improve hydrogen sulfide reaction conversion rate and total sulfur recovery rate.

[0006] The present invention is achieved through the following technical solutions:

[0007] The present invention provides a device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide, comprising an air intake device, a hollow reaction tube, a condenser and a sulfur collecting device connected in sequence;

[0008] The hollow reaction tube is arranged in a heating furnace, and a heat preservation structure is arranged outside the connecting pipe between the hollow reaction tube and the condenser. An inverted catalyst placement tube is arranged in the hollow reaction tube, and a plurality of through holes are opened at the bottom of the catalyst placement tube to communicate with the upper space of the hollow reaction tube. Different catalysts are respectively filled in the catalyst placement tube and 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 arranged 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 thermal insulation material, and a carbon silicon heating rod is arranged inside the heating furnace.

[0011] As a further technical solution of the present invention, a temperature measuring device is arranged in the hollow reaction tube, and the temperature measuring device includes a corundum temperature measuring sleeve and a thermocouple arranged in the corundum temperature measuring sleeve.

[0012] As a further technical solution of the present invention, the thermal 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, a gas outlet pipe is connected to the side of the sulfur collection device, and the gas outlet pipe is connected to the tail gas purification pipe and the reflux pipe through a three-way valve.

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

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

[0017] As a further technical solution of the present invention, the inner wall of the hollow reaction tube is provided with multiple groups of connection holes 1, the side wall of the catalyst placement tube is penetrated by a group of connection holes 2, and both ends of the elastic retaining spring pass through the connection holes 1 and 2 to achieve fixation.

[0018] The present invention also provides a method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide, comprising the following steps:

[0019] S1. Catalyst loading

[0020] According to the catalyst bed height and catalyst dosage requirements, the inverted catalyst placement tube is fixed at a suitable height in the hollow reaction tube, the catalyst A is filled in the upper space of the hollow reaction tube, and the catalyst B is filled in the catalyst placement tube;

[0021] S2. Start the reaction

[0022] The equipment is started, the heating furnace is powered on to increase the temperature, hydrogen sulfide gas is introduced into the hollow reaction tube, the hydrogen sulfide gas passes through the catalyst A and the catalyst B in sequence to react, then flows out from the outlet of the hollow reaction tube, passes through the insulation structure and enters the condenser to be condensed, and sulfur is recovered in the sulfur collection device to obtain sulfur;

[0023] S3, reaction cycle

[0024] Part of the gas flowing out of the sulfur collection device flows back to the hollow reaction tube for secondary reaction, and part of the gas enters the gas chromatography detection device after purification 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. The present invention arranges an inverted catalyst placement tube in the hollow reaction tube, and the height of the catalyst placement tube in the hollow reaction tube can be adjusted as needed, thereby achieving the technical effects of controllable catalyst bed height, controllable ratio of upper and lower catalysts and spatial separation, and can realize multi-stage reaction. By arranging a heat preservation 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. The present invention arranges an inverted catalyst placement tube in the hollow reaction tube to spatially separate the two catalysts and react them in sequence, which can effectively improve the hydrogen sulfide reaction conversion rate and the total sulfur recovery rate. The catalyst placement tube can be adjusted as needed, making it more convenient to control the catalyst bed height, catalyst ratio and dosage. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and should not be regarded as limiting the scope. For those of ordinary skill in the art, other relevant drawings can be obtained based on these drawings without creative work. In the drawings:

[0029] Figure 1 It is a structural schematic diagram of the device of the present invention;

[0030] Figure 2 Schematic diagram of the connection structure between the catalyst placement tube and the hollow reaction tube.

[0031] Marks and corresponding parts names in the attached drawings:

[0032] 1-hydrogen sulfide storage tank, 2-mass flowmeter, 3-heating furnace, 4-hollow reaction tube, 401-connecting hole one, 5-vacuum flange, 6-temperature measuring device, 7-catalyst placement tube, 701-connecting hole two, 702-through hole, 8-carbon silicon heating rod, 9-insulation structure, 10-condenser, 11-sulfur collecting device, 12-three-way valve, 13-reflux pipe, 14-exhaust gas purification pipe, 15-exhaust gas purification device, 16-gas chromatography detection device, 17-elastic retaining spring. DETAILED DESCRIPTION

[0033] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with embodiments and drawings. The exemplary embodiments of the present invention and their description are only used to explain the present invention and are not intended to limit the present invention.

[0034] In the following description, a large number of specific details are set forth in order to provide a thorough understanding of the present invention. However, it is apparent to one of ordinary skill in the art that these specific details are not necessarily employed to practice the present invention. In other embodiments, in order to avoid obscuring the present invention, well-known structures, circuits, materials, or methods are not specifically described.

[0035] Example 1

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

[0037] The hollow reaction tube 4 is arranged in the heating furnace 3, and a heat preservation structure 9 is arranged outside the connecting pipe between the hollow reaction tube 4 and the condenser 10. An inverted catalyst placement tube 7 is arranged in the hollow reaction tube 4. A plurality of through holes 702 are opened at the bottom of the catalyst placement tube 7 to communicate with the upper space of the hollow reaction tube 4. Different catalysts are filled in the catalyst placement tube 7 and the upper space of the hollow reaction tube 4 respectively.

[0038] The present invention arranges an inverted catalyst placement tube 7 in the hollow reaction tube 4, and the height of the catalyst placement tube 7 in the hollow reaction tube 4 can be adjusted as needed, thereby achieving the technical effects of controllable catalyst bed height, controllable ratio of upper and lower catalysts and spatial separation. By arranging a heat preservation structure 9 outside the connecting pipe between the hollow reaction tube 4 and the condenser 10, efficient recovery of product sulfur resources can be achieved and sulfur blockage can be effectively avoided.

[0039] Among them, the air intake device includes a hydrogen sulfide storage tank 1 and a mass flowmeter 2. The hydrogen sulfide storage tank 1 is connected to the hollow reaction tube 4 through an air intake pipe. The mass flowmeter 2 is arranged on the air intake pipe. The mass flowmeter 2 is made of corrosion-resistant material and is used to measure the mass flow of hydrogen sulfide gas.

[0040] Among them, the internal cavity of the heating furnace 3 is filled with insulation material, and a carbon silicon heating rod 8 is arranged inside the heating furnace 3; specifically, the heating furnace 3 is a single-stage vertical, open insulation reaction furnace, and is equipped with an electronic control system, which can accurately control the heating temperature to 300-1600°C. The thickness of the internal cavity insulation layer is greater than 10 cm, and it has high temperature resistance, good heating stability and temperature uniformity. The furnace temperature can be controlled at RT~1600°C, the overshoot temperature is less than 10°C, and it has an over-temperature alarm function.

[0041] The hollow reaction tube 4 is provided with a temperature measuring device 6, which includes a corundum temperature measuring sleeve and a thermocouple arranged in the corundum temperature measuring sleeve. The thermocouple is controlled by a temperature controller. The temperature control range is: room temperature to 1600°C, and the temperature control accuracy is ≤1°C.

[0042] Among them, the insulation structure 9 adopts an electric heating sleeve; since the connection section between the hollow reaction tube 4 and the condenser 10 is most likely to cause sulfur blockage in the pipeline, the present invention designs the connecting pipeline to enlarge the inner diameter and shorten the length and sets the insulation structure 9 for insulation. The pipeline length is 1 to 3 cm, the outer diameter is 1 to 2 cm, and the inner diameter is 0.8 to 1.8 cm. The insulation structure 9 of the pipeline adopts a flexible electric heating sleeve to insulate the pipeline, control the temperature of the gas in the pipeline, avoid high-temperature cooling and rapid cooling, increase the service life of the device, and effectively avoid sulfur cooling and condensation here to block the pipeline.

[0043] The condenser 10 adopts a shell-and-tube condenser 10; specifically, the shell-and-tube condenser 10 has a diameter of 8 to 15 cm and a height of 15 to 20 cm, and contains 6 to 10 heat exchange tube bundles inside. The heat exchange tube bundles are connected to the tube sheets, and the tube sheets are welded to both ends of the shell. The shell is equipped with fluid inlet and outlet pipes. The connections between the tube bundles and the tube sheets and the shell are rigid. Condensate flows outside the heat exchange tube bundle to cool the gas in the tube. The condensate temperature is 10 to 20°C, so that the sulfur vapor is completely cooled and solidified into sulfur in this part.

[0044] Among them, the sulfur collection device 11 is connected to an outlet pipe on the side, and the outlet pipe is connected to the exhaust gas purification pipe 14 and the reflux pipe 13 through a three-way valve 12. The exhaust gas purification pipe 14 is connected to the exhaust gas purification device 15 and the gas chromatography detection device 16 in sequence, and the reflux pipe 13 is connected to the air inlet of the hollow reaction tube 4; the three-way valve 12 is set to control the diversion, 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 circulates to the hollow reaction tube 4 to achieve synchronous detection of the reaction exhaust gas and a secondary reaction before returning to the reaction unit to promote the reaction conversion; specifically, the exhaust gas purification device 15 is built-in quartz wool and calcium chloride to dry and purify the exhaust gas, while avoiding the contamination of the detection system by impurities.

[0045] Among them, Figure 2 As shown, the inner wall of the hollow reaction tube 4 is provided with a plurality of groups of connection holes 401, and the side wall of the catalyst placement tube 7 is penetrated with a group of connection holes 701. Both ends of the elastic retaining spring 17 pass through the connection holes 401 and the connection holes 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, which is sealed by a vacuum flange 5, is hollow at the top and bottom, and is 30cm to 80cm long. The inner diameter of the hollow reaction tube 4 is 1 to 5cm, and the outer diameter is 1.5 to 7cm. The inner wall of the hollow reaction tube 4 is punched to form a connecting hole 401, and the diameter of the connecting hole 401 is 1 to 2mm; the catalyst placement tube 7 is inverted in the hollow reaction tube 4, and 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, and a through hole 702 is punched at the bottom, and the diameter of the through hole 702 is 0.1 to 1mm.

[0047] It should be understood that in order for the catalyst placement tube 7 to separate the upper and lower layers of catalyst, 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, thereby ensuring that the upper catalyst will not enter the interior of the catalyst placement tube 7, thereby achieving physical separation of the two catalysts.

[0048] When the height of the two catalyst beds or the ratio of the catalyst dosage needs to be adjusted, the two ends of the elastic clamp 17 are inserted into the connection hole 2 701 on the side wall of the catalyst placement tube 7, and the catalyst placement tube is moved up and down to the required position. When the height is adjusted and suitable, the two ends of the elastic clamp 17 are inserted into the connection hole 1 401 on the side wall of the hollow reaction tube 4, thereby achieving the fixation of the hollow reaction tube 4 and the catalyst placement tube 7. Figure 2 As shown, the connection holes 401 opened on the side wall of the hollow reaction tube 4 are arranged in multiple rows up and down, so as to facilitate the adjustment of the height of the catalyst placement tube 7.

[0049] Example 2

[0050] This embodiment provides a method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide based on the device of embodiment 1, comprising the following steps:

[0051] S1. Catalyst loading

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

[0053] Catalysts molybdenum sulfide and aluminum oxide are respectively filled in the upper space of the hollow reaction tube and the inside of the catalyst placement tube, and the heights of the two catalyst beds are 8.3 cm and 4.0 cm respectively.

[0054] S2. Start the reaction

[0055] Start the equipment, turn on the power to heat the heating furnace, the temperature of the reaction furnace is 800°C, and introduce a gas with a hydrogen sulfide concentration of 50% into the hollow reaction tube at a gas flow rate of 100 mL / min. The hydrogen sulfide gas reacts with molybdenum sulfide and aluminum oxide in sequence for 120 minutes, and then flows out from the outlet of the hollow reaction tube and passes through an electric heating jacket for insulation (250°C) to enter a condenser for condensation (20°C condensed water), and 6.86 g of sulfur is recovered in a sulfur collection device;

[0056] Among them, the pipe length of the hollow reaction tube outlet and the condenser connection section is 1cm, the outer diameter is 10mm, the flexible electric heating jacket is 8cm long, the internal diameter is 8cm and 1.5cm, and the width is adapted to 3cm. The condenser adopts a shell-and-tube condenser, which contains 12 heat exchange tube bundles.

[0057] S3, reaction cycle

[0058] The gas flows out from the outlet on the side of the sulfur collection device, and the split is controlled. 19 / 20 of the gas flows back to the hollow reaction tube for secondary reaction, and 1 / 20 of the gas enters the gas chromatography detection device after purification to determine that the single-stage conversion rate is 50% and the total recovery rate of sulfur in the circulating reaction is 80%;

[0059] Among them, the gas chromatography detection device selects 9Ft 1 / 8 2mm MolSieve 13X 45 / 60UM, 3Ft 1 / 8 2mmHayeSep Q 80 / 100UM, PLOT Q withPT 3 chromatographic columns, and TCD with EPC detector to achieve simultaneous detection of hydrogen sulfide, hydrogen, organic sulfur, carbon monoxide and other components on the same chromatogram.

[0060] Example 3

[0061] This embodiment provides a method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide based on the device of embodiment 1, comprising the following steps:

[0062] S1. Catalyst loading

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

[0064] Catalysts molybdenum sulfide and aluminum oxide are respectively filled in the upper space of the hollow reaction tube and the inside of the catalyst placement tube, and the heights of the two catalyst beds are 43.4 cm and 36.6 cm respectively.

[0065] S2. Start the reaction

[0066] Start the equipment, turn on the power to heat the heating furnace, the temperature of the reaction furnace is 1000°C, and introduce a gas with a hydrogen sulfide concentration of 50% into the hollow reaction tube, the gas flow rate is 800mL / min, the hydrogen sulfide gas reacts with molybdenum sulfide and aluminum oxide in sequence, the reaction time is 40min, and then flows out from the outlet of the hollow reaction tube, passes through an electric heating jacket for insulation (250°C), enters a condenser for condensation (20°C condensed water), and recovers 21.72g of sulfur in a sulfur collection device;

[0067] Among them, the pipe length of the hollow reaction tube outlet and the condenser connection section is 3cm, the outer diameter is 10mm, the flexible electric heating jacket is 8cm long, the internal diameter is 8cm and 1.5cm, and the width is adapted to 3cm. The condenser adopts a shell-and-tube condenser, which contains 10 heat exchange tube bundles.

[0068] S3, reaction cycle

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

[0070] Among them, the gas chromatography detection device selects 9Ft 1 / 8 2mm MolSieve 13X 45 / 60UM, 3Ft 1 / 8 2mmHayeSep Q 80 / 100UM, PLOT Q withPT 3 chromatographic columns, and TCD with EPC detector to achieve simultaneous detection of hydrogen sulfide, hydrogen, organic sulfur, carbon monoxide and other components on the same chromatogram.

[0071] Example 4

[0072] This embodiment provides a method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide based on the device of embodiment 1, comprising the following steps:

[0073] S1. Catalyst loading

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

[0075] Catalysts molybdenum sulfide and aluminum oxide are respectively filled in the upper space of the hollow reaction tube and the inside of the catalyst placement tube, and the heights of the two catalyst beds are 11.3 cm and 9.2 cm respectively.

[0076] S2. Start the reaction

[0077] Start the equipment, turn on the power to heat the heating furnace, the temperature of the reaction furnace is 1000°C, and introduce a gas with a hydrogen sulfide concentration of 50% into the hollow reaction tube at a gas flow rate of 300 mL / min. The hydrogen sulfide gas reacts with molybdenum sulfide and aluminum oxide in sequence for 40 minutes, and then flows out from the outlet of the hollow reaction tube and passes through an electric heating jacket for insulation (250°C) to enter a condenser for condensation (20°C condensed water), and 8.13 g of sulfur is recovered in a sulfur collection device;

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

[0079] S3, reaction cycle

[0080] The gas flows out from the outlet on the side of the sulfur collection device, and the split is controlled. 19 / 20 of the gas flows back to the hollow reaction tube for secondary reaction, and 1 / 20 of the gas enters the gas chromatography detection device after purification. It is determined that the single-stage conversion rate is 65% and the total recovery rate of sulfur in the cyclic reaction is 95%;

[0081] Among them, the gas chromatography detection device selects 9Ft 1 / 8 2mm MolSieve 13X 45 / 60UM, 3Ft 1 / 8 2mmHayeSep Q 80 / 100UM, PLOT Q withPT 3 chromatographic columns, and TCD with EPC detector to achieve simultaneous detection of hydrogen sulfide, hydrogen, organic sulfur, carbon monoxide and other components on the same chromatogram.

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

[0083] Table 1. Data records related to hydrogen sulfide cracking in Example 2-4

[0084]

[0085]

[0086] Comparative Example

[0087] In this example, based on Example 2, the catalyst placement tube in the hollow reaction tube is removed and the catalyst is directly loaded. The difference is that the catalyst bed height cannot be accurately evaluated and the catalysts are mixed together. The single-stage conversion rate is 45%. Sulfur is recovered and weighed to obtain 5.83g of sulfur. The comparative data of this comparative example and Example 2 are shown in Table 2.

[0088] Table 2. Comparative Examples and Comparative Data of Example 2

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

[0090] From the data comparison of Example 2 and the comparative example, it can be seen that after the catalyst placement tube is removed, the single-stage conversion rate of hydrogen sulfide and the total sulfur recovery rate of the cyclic reaction are both reduced. It can be explained that the setting of the catalyst placement tube spatially separates the two catalysts and reacts them in sequence, which can effectively improve the hydrogen sulfide reaction conversion rate and the total sulfur recovery rate, and the catalyst placement tube can be adjusted as needed, so that it is more convenient to control the catalyst bed height, catalyst ratio and dosage.

[0091] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method 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 in the scope of protection of the present invention.

Claims

1. A device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide, characterized in that: It comprises an air intake device, a hollow reaction tube (4), a condenser (10) and a sulfur collecting device (11) which are connected in sequence; The hollow reaction tube (4) is arranged in the heating furnace (3); a heat-insulating structure (9) is arranged outside the connecting pipe between the hollow reaction tube (4) and the condenser (10); an inverted catalyst placement tube (7) is connected inside the hollow reaction tube (4) via an elastic retaining spring (17); a plurality of through holes (702) are provided at the bottom of the catalyst placement tube (7) and communicate with the upper space of the hollow reaction tube (4); different catalysts are respectively filled inside the catalyst placement tube (7) and the upper space of the hollow reaction tube (4).

2. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that: The air intake 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) via an air intake pipe, and the mass flow meter (2) is arranged on the air intake pipe.

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 heat-insulating material, and a carbon silicon heating rod (8) is arranged inside the heating furnace (3).

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), and 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 thermal insulation structure (9) adopts an electric heating jacket.

6. The device for recovering sulfur by thermal catalytic cracking 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 collecting device (11) is connected to a gas outlet pipeline on its side, and the gas outlet pipeline is connected to a tail gas purification pipe (14) and a reflux pipe (13) via 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 tail gas purification pipe (14) is connected to the tail gas purification device (15) and the gas chromatography detection device (16) in sequence, and the reflux pipe (13) is connected to the air inlet of the hollow reaction tube (4).

9. The device for recovering sulfur by thermal catalytic cracking of hydrogen sulfide according to claim 1, characterized in that: The inner wall of the hollow reaction tube (4) is provided with a plurality of groups of connection holes 1 (401), the side wall of the catalyst placement tube (7) is penetrated by a group of connection holes 2 (701), and the two ends of the elastic retaining spring (17) pass through the connection holes 1 (401) and the connection holes 2 (701) to achieve fixation.

10. A method for recovering sulfur by thermal catalytic cracking of hydrogen sulfide, characterized in that: The following steps are involved: S1. Catalyst loading 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), the catalyst A is filled in the upper space of the hollow reaction tube (4), and the catalyst B is filled in the catalyst placement tube (7); S2. Start the reaction The equipment is started, the heating furnace (3) is powered on to increase the temperature, hydrogen sulfide gas is introduced into the hollow reaction tube (4), the hydrogen sulfide gas passes through the catalyst A and the catalyst B in sequence to react, then flows out from the outlet of the hollow reaction tube (4) through the heat preservation structure (9) and enters the condenser (10) for condensation, and sulfur is recovered in the sulfur collection device (11) to obtain sulfur; S3, reaction cycle A portion of the gas flowing out of the sulfur collecting device (11) flows back to the hollow reaction tube (4) to undergo a secondary reaction, and a portion of the gas enters a gas chromatography detection device (16) after being purified to determine a single-stage conversion rate.

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