Fischer-Tropsch synthesis reaction device and treatment method for oxidation inactivation of iron-based catalyst by adopting Fischer-Tropsch synthesis reaction device
By combining dynamic cooking and static cooking methods in the Fischer Tropsch synthesis reaction device, the iron-based catalyst is oxidatively deactivated, which solves the problem of catalyst spontaneous combustion after the Fischer Tropsch synthesis reaction process, and achieves a safe and efficient wax cleaning process.
Patent Information
- Application Number
- CN202411706841.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-26
- Publication Date
- 2025-03-28
- Estimated Expiration
- 2044-11-26
AI Technical Summary
After the Fischer-Tropsch synthesis reaction process is handed over, the iron-based catalyst is exposed and has high activity, resulting in a high risk of spontaneous combustion and it is difficult for the prior art to effectively deal with it.
A Fischer Tropsch synthesis reaction device is designed, including a Fischer Tropsch synthesis reactor, heat exchange tube, steam drum and cyclone separator. The iron-based catalyst is oxidatively deactivated by a combination of dynamic cooking and static cooking. The air is passed through the manhole at the bottom to burn the uninactivated catalyst, and the gas state and CO content are detected through the manhole at the top to determine whether to perform artificial wax cleaning.
It effectively reduces the risk of spontaneous combustion of iron-based catalysts, reduces the difficulty and time of artificial wax cleaning, and improves safety and efficiency.
Smart Images

Figure CN119701791A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of Fischer-Tropsch synthesis reaction, and in particular to a Fischer-Tropsch synthesis reaction device and a method for treating oxidation deactivation of an iron-based catalyst using the same. Background Art
[0002] Synthesis gas (CO and H2) undergoes Fischer-Tropsch synthesis reaction under iron-based catalysts and certain conditions to produce wax, heavy hydrocarbons and light hydrocarbons. It is one of the indirect coal liquefaction technologies. The stable Fischer-Tropsch synthesis iron-based catalyst exists in an oxidized form. It is activated in the catalyst reduction reactor to convert the oxidized iron-based catalyst into iron carbide. Therefore, it is the iron carbide that actually undergoes the Fischer-Tropsch synthesis reaction. During the process handover of the Fischer-Tropsch reactor, when the manhole is opened, a large amount of catalyst containing wax oil attached to the heat exchange tubes and the top cyclone separator will spontaneously combust when it encounters air. In order to prevent the fire from spreading and burning the internal parts, it is necessary to enter the reactor for manual cleaning, which makes the cleaning extremely difficult. At the same time, during the cleaning process, the carbon monoxide released by combustion can easily cause personnel poisoning. Therefore, the risk is extremely high and the process handover time is long.
[0003] The prior art still has the following problems:
[0004] 1) After the Fischer-Tropsch reactor process is completed, it enters the cooking stage. However, the partial pressure of the circulating nitrogen and steam entering the reactor is low, which cannot fully oxidize and extinguish the catalyst. In addition, the steam has a short residence time in the Fischer-Tropsch reactor, and the contact time with the residual catalyst is insufficient, so the structure of the catalyst is not destroyed.
[0005] 2) During the cooking period, most of the steam in the Fischer-Tropsch reactor still exists in the form of steam, which cannot destroy the activity of the catalyst. Instead, it evaporates the wax oil that originally wrapped the catalyst, exposing the catalyst completely. After the manhole is opened, the catalyst containing the wax oil comes into contact with the air and spontaneously ignites.
[0006] 3) The residual catalyst of the Fischer-Tropsch reactor is mainly concentrated on the cyclone separator and heat exchange tubes at the top, but after opening the manhole, artificial watering cannot flush the catalyst above the cyclone separator opposite the manhole.
[0007] 4) The air volume for catalyst passivation was not solidified and the ventilation was too large, causing the residual exposed catalyst to spontaneously combust.
[0008] Therefore, a process is urgently needed to solve the problem that the Fischer-Tropsch synthesis catalyst is exposed and its activity is still high after the Fischer-Tropsch reaction process is handed over, resulting in spontaneous combustion after the manhole is opened. Summary of the invention
[0009] The main purpose of the present invention is to provide a Fischer-Tropsch synthesis reaction device and a method for treating the oxidative deactivation of an iron-based catalyst using the same, so as to solve the problem in the prior art that the Fischer-Tropsch synthesis iron-based catalyst is exposed and has high activity after the handover process of the Fischer-Tropsch synthesis reaction process, resulting in spontaneous combustion after the manhole is opened.
[0010] To achieve the above-mentioned object, according to one aspect of the present invention, a Fischer-Tropsch synthesis reaction device is provided, the Fischer-Tropsch synthesis reaction device comprising: a Fischer-Tropsch synthesis reactor, a heat exchange tube, a steam drum and a cyclone separator, wherein the Fischer-Tropsch synthesis reactor provides a reaction site for a Fischer-Tropsch synthesis reaction product system comprising an iron-based catalyst and wax; the Fischer-Tropsch synthesis reactor is used for performing a first oxidation deactivation on the iron-based catalyst by dynamic cooking to obtain a first product, and for performing a second oxidation deactivation on the iron-based catalyst in the first product by static cooking to obtain a product comprising wax and the iron-based catalyst; The heavy products of the catalytic agent and the gas to be discharged; the Fischer-Tropsch synthesis reactor is provided with a heat exchange tube, which includes an upper heat exchange tube and a lower heat exchange tube; the heat exchange tube is used to control the temperature in the Fischer-Tropsch synthesis reactor; the steam drum is arranged outside the Fischer-Tropsch synthesis reactor, and the steam drum includes an upper steam drum and a lower steam drum, the upper steam drum is connected with the upper heat exchange tube, and the lower steam drum is connected with the lower heat exchange tube, the upper steam drum is used to control the temperature of the upper section of the Fischer-Tropsch synthesis reactor, and the lower steam drum is used to control the temperature of the lower section of the Fischer-Tropsch synthesis reactor; the steam drum is used to heat the upper heat exchange tube during static cooking. The wax and iron-based catalyst on the tube are heated and melted to obtain heavy products; the temperature of the upper section of the Fischer-Tropsch synthesis reactor is higher than that of the lower section of the Fischer-Tropsch synthesis reactor; a plurality of cyclone separators 4, each cyclone separator 4 is close to the top of the Fischer-Tropsch synthesis reactor 1 and is arranged in the Fischer-Tropsch synthesis reactor 1, the plurality of cyclone separators 4 are arranged in a horizontal ring, and each cyclone separator 4 has a certain horizontal distance from the inner side wall of the Fischer-Tropsch synthesis reactor 1; the side wall of the top of the Fischer-Tropsch synthesis reactor has a plurality of desalted water inlets, each desalted water inlet is used to introduce desalted water to flush the iron-based catalyst on the cyclone separator to destroy and deactivate the iron-based catalyst; the Fischer-Tropsch synthesis reactor also includes a top manhole and a bottom manhole, the bottom manhole is used to introduce air into the Fischer-Tropsch synthesis reactor and burn the non-deactivated iron-based catalyst, and the top manhole is used to introduce water into the Fischer-Tropsch synthesis reactor to cool the exhaust gas to obtain the cooled exhaust gas; the top temperature of the Fischer-Tropsch synthesis reactor and the gas state of the exhaust gas after cooling, the composition of the exhaust gas after cooling and the CO content therein are detected to determine whether to perform manual wax cleaning.
[0011] Furthermore, a nitrogen pipeline and a circulating nitrogen pipeline are also provided at the bottom of the Fischer-Tropsch synthesis reactor; a first steam cooking line is connected to the pipeline of the nitrogen pipeline; a bottom catalyst feeding port is also provided at the bottom of the Fischer-Tropsch synthesis reactor, and a bottom steam cooking line is connected to the pipeline of the bottom catalyst feeding port; the first steam cooking line is used to transport the first steam into the Fischer-Tropsch synthesis reactor; the circulating nitrogen pipeline is used to transport the first nitrogen into the Fischer-Tropsch synthesis reactor, and the bottom steam cooking line is used to transport the second steam into the Fischer-Tropsch synthesis reactor; the first steam is mixed with the first nitrogen and then used with the second steam for dynamic cooking; preferably, the first nitrogen is used to replace the gas in the Fischer-Tropsch synthesis reactor; the first steam and the second steam are used for the first oxidation deactivation of the iron-based catalyst; preferably, the nominal diameter of the first steam cooking line is 80 mm, and / or, the pressure of the first steam is 1.0 MPa, and / or, the pressure of the second steam is 1.0 MPa, and / or, the temperature of the first nitrogen is 110-120°C, and / or, the nominal diameter of the bottom steam cooking line is 40 mm.
[0012] Furthermore, an upper catalyst unloading port, a middle catalyst unloading port and a lower catalyst unloading port are sequentially arranged on the outer side wall of the Fischer-Tropsch synthesis reactor along the axial direction of the Fischer-Tropsch synthesis reactor, and the pipelines of the upper catalyst unloading port, the middle catalyst unloading port and the lower catalyst unloading port are respectively connected with an upper steam cooking pipeline, a middle steam cooking pipeline and a lower steam cooking pipeline, and the upper steam cooking pipeline, the middle steam cooking pipeline, the lower steam cooking pipeline and the bottom steam cooking line are used to transport the third steam into the Fischer-Tropsch synthesis reactor for static cooking; and / or, when static cooking is carried out, the pressure in the Fischer-Tropsch synthesis reactor is 0.1-0.15MPa, and the nominal diameters of the upper steam cooking pipeline, the middle steam cooking pipeline and the lower steam cooking pipeline are each independently 40mm.
[0013] Furthermore, the inlet pipelines of the upper steam drum and the lower steam drum are respectively connected with the upper steam drum steam pipeline and the lower steam drum steam pipeline; the pressures of the steam transported by the upper steam drum steam pipeline and the lower steam drum steam pipeline are independently 5.4 MPa; the temperature of the lower section of the Fischer-Tropsch synthesis reactor is 140-150°C, and the temperature of the upper section of the Fischer-Tropsch synthesis reactor is 180-200°C.
[0014] Furthermore, the Fischer-Tropsch synthesis reaction device further comprises a compressor, which is connected to a circulating nitrogen pipeline, and the compressor is used to circulate the first nitrogen during the dynamic cooking process; and / or the nitrogen pipeline is used to provide a second nitrogen to the Fischer-Tropsch synthesis reactor for cooling, and the feed amount of the second nitrogen is 8000-9000 Nm 3 / h; and / or, the Fischer-Tropsch synthesis reaction device also includes a pressure tank connected to the Fischer-Tropsch synthesis reactor, and the heavy product is pressed into the pressure tank through the lower catalyst unloading port.
[0015] Furthermore, the combustible gas in the first product is discharged into a flare system connected to the Fischer-Tropsch synthesis reactor.
[0016] Further, the opening angles of the top manhole and the bottom manhole are independently 10 to 90°; and / or, after the desalted water is introduced for flushing, the temperature of the top of the Fischer-Tropsch synthesis reactor is tested, and when the temperature of the top of the Fischer-Tropsch synthesis reactor is ≥70°C, the opening angle of the top manhole is opened to 90°, and water is introduced into the Fischer-Tropsch synthesis reactor through the top manhole while the second nitrogen is introduced to cool it down for 20 to 25 minutes, and then the introduction of the second nitrogen is stopped and the opening angle of the bottom manhole is opened to 10 to 15°, and the top temperature of the Fischer-Tropsch synthesis reactor and the gas state of the exhaust gas after cooling, and the gas state of the exhaust gas after cooling are measured. The composition of the gas to be discharged and the content of CO therein are first tested; the qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor is ≤40°C, and the gas to be discharged after cooling is in a water vapor state and does not contain flue gas, and the content of CO in the gas to be discharged after cooling is <25ppm; when the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor is ≥50°C, the gas to be discharged after cooling is in a water vapor state and contains flue gas, and the content of CO in the gas to be discharged after cooling is ≥25ppm, water is introduced into the Fischer-Tropsch synthesis reactor for 10 minutes for cooling every 30 minutes and the cooling is continued for 2 hours until the test result is qualified; Subsequently, the opening angle of the bottom manhole is increased by 15 to 20 degrees each time until the opening angle is 90 degrees. If the test result is qualified, the Fischer-Tropsch synthesis reactor is entered through the top and bottom manholes for manual wax removal; and in the process of opening the bottom manhole angle, before each time the bottom manhole is opened to a new angle, ensure that the test result is qualified, otherwise, water is introduced into the Fischer-Tropsch synthesis reactor for 10 minutes every 30 minutes to cool it down and continue for 2 hours until the test result is qualified; when the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor is less than 50°C, and the wastewater to be discharged after cooling down is discharged, the wastewater is discharged from the reactor and the top temperature is less than 50°C. The gas is in a water vapor state and does not contain flue gas. When the CO content in the exhaust gas after cooling is <25ppm, the opening angle of the bottom manhole is increased by 15 to 20° each time until the opening angle is 90°. If the test result is qualified, enter the Fischer-Tropsch synthesis reactor through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, each time before the bottom manhole opens a new angle, ensure that the test result is qualified, otherwise water is introduced into the Fischer-Tropsch synthesis reactor for 10 minutes for cooling every 30 minutes and continued for 2 hours until the test result is qualified.
[0017] According to another aspect of the present invention, a method for treating the oxidative deactivation of an iron-based catalyst using the above-mentioned Fischer-Tropsch synthesis reaction device is provided, the method comprising: performing a first oxidative deactivation on the iron-based catalyst in the Fischer-Tropsch synthesis reaction product system including the iron-based catalyst and wax using dynamic cooking in the Fischer-Tropsch synthesis reactor to obtain a first product; performing a second oxidative deactivation on the iron-based catalyst in the first product using static cooking to obtain a heavy product including the wax and the iron-based catalyst and a gas to be discharged; during the static cooking period, heating and melting the wax and the iron-based catalyst on the upper heat exchange tubes to obtain a heavy product. the temperature of the upper section of the Fischer-Tropsch synthesis reactor is higher than the temperature of the lower section of the Fischer-Tropsch synthesis reactor; the iron-based catalyst on the cyclone separator is washed with desalted water to destroy and deactivate the iron-based catalyst; air is introduced into the Fischer-Tropsch synthesis reactor through the bottom manhole to burn the non-deactivated iron-based catalyst, and water is introduced into the Fischer-Tropsch synthesis reactor through the top manhole to cool the exhaust gas to obtain the cooled exhaust gas; and whether to perform artificial wax cleaning is determined by detecting the top temperature of the Fischer-Tropsch synthesis reactor and the gas state of the exhaust gas after cooling, the composition of the exhaust gas after cooling and the CO content therein.
[0018] Furthermore, when the concentration of combustible gas in the first product is less than 5LEL%, the compressor is stopped for 2 to 3 hours and static cooking is carried out; and / or, the dynamic cooking time is 12 to 16 hours, the dynamic cooking temperature is 150 to 160°C, and / or, the static cooking time is 14 to 18 hours, and / or, the static cooking temperature is 150 to 180°C; and / or, the amount of desalted water introduced is 10 to 20 tons / hour.
[0019] Further, after the desalted water is passed for flushing, the temperature at the top of the Fischer-Tropsch synthesis reactor is tested. When the temperature at the top of the Fischer-Tropsch synthesis reactor is ≥70°C, the opening angle of the top manhole is opened to 90°, and water is passed into the Fischer-Tropsch synthesis reactor through the top manhole while the second nitrogen is passed for cooling for 20 to 25 minutes. Then, the second nitrogen is stopped and the opening angle of the bottom manhole is opened to 10 to 15°. The top temperature of the Fischer-Tropsch synthesis reactor and the gas state of the gas to be exhausted after cooling, the composition of the gas to be exhausted after cooling, and the CO content therein are first detected; The qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor is ≤40°C, and the gas to be discharged after cooling is in a water vapor state and does not contain flue gas, and the CO content in the gas to be discharged after cooling is <25ppm; when the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor is ≥50°C, the gas to be discharged after cooling is in a water vapor state and contains flue gas, and the CO content in the gas to be discharged after cooling is ≥25ppm, water is introduced into the Fischer-Tropsch synthesis reactor for 10 minutes for cooling every 30 minutes and continued for 2 hours until the test result is qualified; then the opening angle of the bottom manhole is adjusted by 1 / 4 each time. Increase the opening angle by 15 to 20° until the opening angle is 90°. If the test result is qualified, enter the Fischer-Tropsch synthesis reactor through the top manhole and the bottom manhole for manual wax removal; and in the process of opening the bottom manhole, before each time the bottom manhole opens a new angle, ensure that the test result is qualified. Otherwise, water is introduced into the Fischer-Tropsch synthesis reactor for 10 minutes every 30 minutes to cool it down and continue for 2 hours until the test result is qualified. When the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor is less than 50°C, and the gas to be discharged after cooling is in a water vapor state, Excluding flue gas, when the CO content in the exhaust gas after cooling is <25ppm, the opening angle of the bottom manhole is increased by 15-20° each time until the opening angle is 90°. If the test result is qualified, enter the Fischer-Tropsch synthesis reactor through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, each time before the bottom manhole opens a new angle, ensure that the test result is qualified, otherwise water is introduced into the Fischer-Tropsch synthesis reactor for 10 minutes for cooling every 30 minutes and continued for 2 hours until the test result is qualified.
[0020] By applying the technical solution of the present invention, the present application provides a Fischer-Tropsch synthesis reaction device for the scenario of oxidative deactivation of iron-based catalysts in the Fischer-Tropsch synthesis reaction. By adding static cooking on the basis of dynamic cooking in the Fischer-Tropsch synthesis reactor, the iron-based catalyst and wax attached to the upper heat exchange tubes in the Fischer-Tropsch synthesis reactor can be dropped to the bottom of the Fischer-Tropsch synthesis reactor under the action of gravity and pressed out, thereby reducing the amount of manual wax removal. At the same time, static cooking has a higher degree of damage to the iron-based catalyst. The iron-based catalyst on the cyclone separator in the Fischer-Tropsch synthesis reactor is rinsed with desalted water, which can also cool the Fischer-Tropsch synthesis reactor, so that the desalted water vaporizes during the falling process to form water mist and contacts the iron-based catalyst on the top of the cyclone separator, and the activity of the iron-based catalyst remaining on the top of the cyclone separator is destroyed again, and the degree of destruction is higher. Air is introduced through the bottom manhole, so that the non-deactivated iron-based catalyst can also burn at a lower temperature, thereby avoiding spontaneous combustion during manual wax removal and causing casualties. After cooling the Fischer-Tropsch synthesis reactor through the top manhole and introducing air through the bottom manhole, the temperature at the top of the Fischer-Tropsch synthesis reactor and the gas state of the gas to be exhausted after cooling discharged from the top manhole, the composition of the gas to be exhausted after cooling and the CO content therein are detected, so as to accurately judge whether manual wax removal can be performed. The Fischer-Tropsch synthesis reaction device of the present invention can achieve multiple destruction of the structure of the remaining iron-based catalyst that has not been deactivated, and can greatly reduce the risk of casualties of personnel performing manual wax removal during the rescue process. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The drawings constituting a part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:
[0022] Figure 1 A schematic diagram of the Fischer-Tropsch synthesis reaction device of the present application is shown.
[0023] Among them, the above drawings include the following reference numerals:
[0024] 1. Fischer-Tropsch synthesis reactor; 2. Heat exchange tubes; 3. Steam drum; 4. Cyclone separator; 5. Pressure tank; 21. Upper heat exchange tubes; 22. Lower heat exchange tubes; 31. Upper steam drum; 32. Lower steam drum; A-1. First steam cooking line; A-2. Bottom steam cooking line; A-3. Upper steam cooking pipeline; A-4. Middle steam cooking pipeline; A-5. Lower steam cooking pipeline; A-6. Upper steam drum steam pipeline; A-7. Lower steam drum steam pipeline; B-1. Circulating nitrogen pipeline; B-2. Nitrogen pipeline; C-1. Bottom catalyst feeding port; C-2. Upper catalyst discharge port; C-3. Middle catalyst discharge port; C-4. Lower catalyst discharge port; D-1. First desalted water valve; D-2. Second desalted water valve; D-3. Third desalted water valve. DETAILED DESCRIPTION
[0025] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.
[0026] As analyzed in the background technology of the present application, in the prior art, the iron-based catalyst for Fischer-Tropsch synthesis is exposed after the Fischer-Tropsch synthesis reaction process and has high activity, which leads to spontaneous combustion after the manhole is opened. In order to solve the above problem, the present application provides a Fischer-Tropsch synthesis reaction device and a method for treating the oxidation deactivation of the iron-based catalyst using the same.
[0027] In a typical embodiment of the present application, a Fischer-Tropsch synthesis reaction device is provided, such as Figure 1As shown, the Fischer-Tropsch synthesis reaction device comprises: a Fischer-Tropsch synthesis reactor 1, a heat exchange tube 2, a steam drum 3 and a cyclone separator 4. The Fischer-Tropsch synthesis reactor 1 provides a reaction place for a Fischer-Tropsch synthesis reaction product system including an iron-based catalyst and wax; the Fischer-Tropsch synthesis reactor 1 is used to perform a first oxidation deactivation on the iron-based catalyst by dynamic cooking to obtain a first product, and to perform a second oxidation deactivation on the iron-based catalyst in the first product by static cooking to obtain a heavy product including wax and the iron-based catalyst and a gas to be discharged; the Fischer-Tropsch synthesis reactor 1 is provided with a heat exchange tube 2, the heat exchange tube 2 includes an upper heat exchange tube 21 and a lower heat exchange tube 22; the heat exchange tube 2 is used to control the temperature in the Fischer-Tropsch synthesis reactor 1; the steam drum 3 is arranged outside the Fischer-Tropsch synthesis reactor 1, and the steam drum 3 includes an upper steam drum 31 and a lower steam drum 32, the upper steam drum 31 is connected to the upper heat exchange tube 21, and the lower steam drum 32 is connected to the lower heat exchange tube 22, the upper steam drum 31 is used to control the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1, and the lower steam drum 32 is used to control the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1; the steam drum 3 is used to heat the upper heat exchange tube during static cooking. The wax and iron-based catalyst on 21 are heated and melted to obtain a heavy product; the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 is higher than the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1; a plurality of cyclone separators 4, each cyclone separator 4 is close to the top of the Fischer-Tropsch synthesis reactor 1 and is arranged in the Fischer-Tropsch synthesis reactor 1, and the plurality of cyclone separators 4 are arranged in a horizontal ring shape, and each cyclone separator 4 has a certain horizontal distance from the inner side wall of the Fischer-Tropsch synthesis reactor 1; the side wall of the top of the Fischer-Tropsch synthesis reactor 1 has a plurality of desalted water inlets, and each desalted water inlet is used to pass desalted water The iron-based catalyst on the cyclone separator 4 is flushed to destroy and deactivate the iron-based catalyst; the Fischer-Tropsch synthesis reactor 1 also includes a top manhole and a bottom manhole, the bottom manhole is used to introduce air into the Fischer-Tropsch synthesis reactor 1 and burn the non-deactivated iron-based catalyst, and the top manhole is used to introduce water into the Fischer-Tropsch synthesis reactor 1 to cool the gas to be exhausted, so as to obtain the gas to be exhausted after cooling; the top temperature of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling, the composition of the gas to be exhausted after cooling and the CO content therein are detected to determine whether manual wax cleaning is performed.
[0028] The present application provides a Fischer-Tropsch synthesis reaction device for the scenario of oxidative deactivation of iron-based catalysts in the Fischer-Tropsch synthesis reaction. By adding static cooking on the basis of dynamic cooking in the Fischer-Tropsch synthesis reactor 1, the iron-based catalyst and wax attached to the upper heat exchange tubes 21 in the Fischer-Tropsch synthesis reactor 1 can be dropped to the bottom of the Fischer-Tropsch synthesis reactor 1 under the action of gravity and pressed out, thereby reducing the amount of manual wax removal. At the same time, static cooking has a higher degree of damage to the iron-based catalyst. The iron-based catalyst on the cyclone separator 4 in the Fischer-Tropsch synthesis reactor 1 is flushed with desalted water, which can not only flush the iron-based catalyst attached to the cyclone separator 4, but also play a role in cooling the Fischer-Tropsch synthesis reactor 1, so that the desalted water vaporizes in the process of falling to form water mist and contacts the iron-based catalyst on the top of the cyclone separator 4, and the activity of the iron-based catalyst remaining on the top of the cyclone separator 4 is destroyed again, and the degree of destruction is higher. Air is introduced through the bottom manhole, so that the non-deactivated iron-based catalyst can also burn at a lower temperature, thereby avoiding spontaneous combustion during manual wax removal and causing casualties. After cooling the Fischer-Tropsch synthesis reactor 1 through the top manhole and introducing air through the bottom manhole, the temperature at the top of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling discharged from the top manhole, the composition of the gas to be exhausted after cooling and the CO content therein are detected, and it is possible to accurately determine whether to perform manual wax removal. The Fischer-Tropsch synthesis reaction device of the present invention can achieve multiple destruction of the structure of the remaining iron-based catalyst that has not been deactivated, and can greatly reduce the risk of casualties in the rescue process when performing manual wax removal.
[0029] In one embodiment of the present application, a nitrogen pipeline and a circulating nitrogen pipeline are further provided at the bottom of the Fischer-Tropsch synthesis reactor 1; a first steam cooking line is connected to the pipeline of the nitrogen pipeline; a bottom catalyst feeding port is also provided at the bottom of the Fischer-Tropsch synthesis reactor 1, and a bottom steam cooking line is connected to the pipeline of the bottom catalyst feeding port; the first steam cooking line is used to transport the first steam into the Fischer-Tropsch synthesis reactor 1; the circulating nitrogen pipeline is used to transport the first nitrogen into the Fischer-Tropsch synthesis reactor 1, and the bottom steam cooking line is used to transport the second steam into the Fischer-Tropsch synthesis reactor 1 ; The first steam is mixed with the first nitrogen and then used with the second steam for dynamic cooking; preferably, the first nitrogen is used to replace the gas in the Fischer-Tropsch synthesis reactor 1; the first steam and the second steam are used for a first oxidation deactivation of the iron-based catalyst; preferably, the nominal diameter of the first steam cooking line is 80 mm, and / or the pressure of the first steam is 1.0 MPa, and / or the pressure of the second steam is 1.0 MPa, and / or the temperature of the first nitrogen is 110-120°C, and / or the nominal diameter of the bottom steam cooking line is 40 mm.
[0030] Adding the first steam cooking line of the above specifications helps to increase the steam volume by more than 30%, thereby helping to increase the partial pressure of the steam. At the same time, it is more reasonable to set the first steam cooking line at the bottom of the Fischer-Tropsch synthesis reactor 1 to introduce the first steam, and mix the first steam with the first nitrogen before the distributor. After being distributed by the distributor, the mixed gas is more uniform, thereby further increasing the content of free water, and further enhancing the destructiveness to the iron-based catalyst.
[0031] In one embodiment of the present application, an upper catalyst discharge port, a middle catalyst discharge port and a lower catalyst discharge port are sequentially arranged on the outer side wall of the Fischer-Tropsch synthesis reactor 1 along the axial direction of the Fischer-Tropsch synthesis reactor 1, and the pipelines of the upper catalyst discharge port, the middle catalyst discharge port and the lower catalyst discharge port are respectively connected with an upper steam cooking pipeline, a middle steam cooking pipeline and a lower steam cooking pipeline, and the upper steam cooking pipeline, the middle steam cooking pipeline, the lower steam cooking pipeline and the bottom steam cooking line are used to transport the third steam into the Fischer-Tropsch synthesis reactor 1 for static cooking; and / or, when static cooking is performed, the pressure in the Fischer-Tropsch synthesis reactor 1 is 0.1-0.15MPa, and the nominal diameters of the upper steam cooking pipeline, the middle steam cooking pipeline and the lower steam cooking pipeline are each independently 40mm.
[0032] Preferably, the content of the third steam in the static cooking process is regulated by the upper steam cooking line, the middle steam cooking line, the lower steam cooking line and the bottom steam cooking line, and the pressure in the Fischer-Tropsch synthesis reactor 1 is controlled within the above range, which helps to quickly deactivate the exposed but still active iron-based catalyst and melt the iron-based catalyst containing wax oil attached to the upper heat exchange tubes 21 and then fall back to the bottom of the Fischer-Tropsch synthesis reactor 1.
[0033] In one embodiment of the present application, the inlet pipelines of the upper steam drum 31 and the lower steam drum 32 are respectively connected with the upper steam drum steam pipeline and the lower steam drum steam pipeline; the pressures of the steam transported by the upper steam drum steam pipeline and the lower steam drum steam pipeline are independently 5.4 MPa; the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1 is 140-150°C, and the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 is 180-200°C.
[0034] It is preferred to control the pressure of the steam transported by the upper steam drum pipeline and the lower steam drum pipeline into the upper steam drum 31 and the lower steam drum 32 respectively, as well as the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 and the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1 within the above-mentioned range, which helps to cause the iron-based catalyst and wax attached to the upper heat exchange tubes 21 in the Fischer-Tropsch synthesis reactor 1 to fall to the bottom of the Fischer-Tropsch synthesis reactor 1 under the action of gravity and be pressed out, thereby reducing the amount of manual wax cleaning, and at the same time helps to further increase the degree of damage to the iron-based catalyst.
[0035] In one embodiment of the present application, the Fischer-Tropsch synthesis reaction device further includes a compressor, which is connected to a circulating nitrogen pipeline, and the compressor is used to circulate the first nitrogen during the dynamic cooking process; and / or, the nitrogen pipeline is used to provide a second nitrogen to the Fischer-Tropsch synthesis reactor 1 for cooling, and the feed amount of the second nitrogen is 8000-9000Nm 3 / h; and / or, the Fischer-Tropsch synthesis reaction device also includes a pressure tank, and the heavy product is pressed into the pressure tank through the lower catalyst discharge port.
[0036] Preferably, the compressor circulates the first nitrogen, which helps to fully replace the gas in the Fischer-Tropsch synthesis reactor 1 during the dynamic cooking process. Preferably, the medium-pressure second nitrogen gas introduced into the bottom of the Fischer-Tropsch synthesis reactor 1 is controlled to further improve the cooling effect.
[0037] In one embodiment of the present application, the Fischer-Tropsch synthesis reaction device further comprises a pressure tank connected to the Fischer-Tropsch synthesis reactor 1, and the heavy product is pressed into the pressure tank through the lower catalyst discharge port.
[0038] By pressing the heavy product into the pressure tank, it helps to further reduce the amount of manual wax removal. At the same time, before the heavy product is pressed into the pressure tank, the pressure tank is equipped with a waste catalyst recovery tank with a stirring device. The tank body is provided with an external coil heating at a temperature of 160-180°C. The stirring device helps to evaporate and dehydrate the heavy product. Evaporation and dehydration help to minimize sudden boiling in the process of recovering waste iron-based catalysts containing wax.
[0039] In one embodiment of the present application, the combustible gas in the first product is discharged into a flare system connected to the Fischer-Tropsch synthesis reactor 1 .
[0040] Preferably, the combustible gas in the first product is discharged into a flare system connected to the Fischer-Tropsch synthesis reactor 1, which helps to reduce the concentration of the combustible gas in the gas to be discharged, thereby avoiding the explosion of the combustible gas as much as possible and thus improving safety.
[0041] In one embodiment of the present application, the opening angles of the top manhole and the bottom manhole are independently 10 to 90°; and / or, after the desalted water is introduced for flushing, the temperature at the top of the Fischer-Tropsch synthesis reactor 1 is tested. When the temperature at the top of the Fischer-Tropsch synthesis reactor 1 is ≥70°C, the opening angle of the top manhole is opened to 90°, and water is introduced into the Fischer-Tropsch synthesis reactor 1 through the top manhole while the second nitrogen is introduced to cool it down for 20 to 25 minutes, and then the introduction of the second nitrogen is stopped and the opening angle of the bottom manhole is opened to 10 to 15°, and the top temperature of the Fischer-Tropsch synthesis reactor 1 and the gas to be exhausted after cooling are controlled. The first test is performed on the state, the composition of the gas to be discharged after cooling, and the content of CO therein; the qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is ≤40°C, and the gas to be discharged after cooling is in a water vapor state and does not contain flue gas, and the content of CO in the gas to be discharged after cooling is <25ppm; when the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is ≥50°C, the gas to be discharged after cooling is in a water vapor state and contains flue gas, and the content of CO in the gas to be discharged after cooling is ≥25ppm, water is introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes for cooling every 30 minutes and the cooling is continued for 2 hours until the test result is Qualified state; then the opening angle of the bottom manhole is increased by 15 to 20 degrees each time until the opening angle is 90 degrees. If the test result is qualified, enter the Fischer-Tropsch synthesis reactor 1 through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, before each time the bottom manhole opens a new angle, ensure that the test result is qualified. Otherwise, water is introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes every 30 minutes to cool it down and continue for 2 hours until the test result is qualified; when the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is less than 50°C, and the temperature is lowered The gas to be discharged is in a water vapor state and does not contain flue gas. When the CO content in the gas to be discharged after cooling is <25ppm, the opening angle of the bottom manhole is increased by 15 to 20° each time until the opening angle is 90°. If the test result is qualified, enter the Fischer-Tropsch synthesis reactor 1 through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, each time before the bottom manhole opens a new angle, ensure that the test result is qualified, otherwise water is introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes for cooling every 30 minutes and continued for 2 hours until the test result is qualified.
[0042] By controlling the opening angles of the top manhole and the bottom manhole to adjust the amount of water and nitrogen introduced, it is helpful to cool down the Fischer-Tropsch synthesis reactor 1 and detect the temperature at the top of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling and discharged from the top manhole, the composition of the gas to be exhausted after cooling and whether the CO content therein is in a qualified state, thereby helping to further accurately determine whether manual wax cleaning can be performed and effectively clean the wax accumulated inside the Fischer-Tropsch synthesis reactor 1, while ensuring personnel safety. Among them, when the opening angle of the bottom manhole is 90° for the last detection, continuous detection for 2 hours is required, during which detection is performed every 10 minutes or 30 minutes, and the CO content is less than 25ppm, thereby ensuring the safety of the manual wax cleaning process.
[0043] In a typical embodiment of the present application, a method for treating the oxidative deactivation of an iron-based catalyst using the above-mentioned Fischer-Tropsch synthesis reaction device is provided, and the method comprises: performing a first oxidative deactivation on the iron-based catalyst in the Fischer-Tropsch synthesis reaction product system including the iron-based catalyst and wax by dynamic cooking in the Fischer-Tropsch synthesis reactor 1 to obtain a first product; performing a second oxidative deactivation on the iron-based catalyst in the first product by static cooking to obtain a heavy product including the wax and the iron-based catalyst and a gas to be discharged; during the static cooking, heating and melting the wax and the iron-based catalyst on the upper heat exchange tubes 21 to obtain a heavy product; product; the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 is higher than the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1; the iron-based catalyst on the cyclone separator 4 is flushed with desalted water to destroy and deactivate the iron-based catalyst; air is introduced into the Fischer-Tropsch synthesis reactor 1 through the bottom manhole and the non-deactivated iron-based catalyst is burned, and water is introduced into the Fischer-Tropsch synthesis reactor 1 through the top manhole to cool the exhaust gas to obtain the cooled exhaust gas; by detecting the top temperature of the Fischer-Tropsch synthesis reactor 1 and the gas state of the exhaust gas after cooling, the composition of the exhaust gas after cooling and the CO content therein to determine whether to perform manual wax cleaning.
[0044] The present application is aimed at the scenario of oxidative deactivation of iron-based catalysts in the Fischer-Tropsch synthesis reaction. By adding static cooking on the basis of dynamic cooking, the iron-based catalyst and wax attached to the upper heat exchange tubes 21 in the Fischer-Tropsch synthesis reactor 1 can be dropped to the bottom of the Fischer-Tropsch synthesis reactor 1 and pressed out under the action of gravity, thereby reducing the amount of manual wax removal. At the same time, static cooking has a higher degree of damage to the iron-based catalyst. Flushing the iron-based catalyst on the cyclone separator 4 in the Fischer-Tropsch synthesis reactor 1 with desalted water can also cool the Fischer-Tropsch synthesis reactor 1, so that the desalted water vaporizes and destroys the activity of the iron-based catalyst again, and the degree of damage is higher. Air is introduced through the bottom manhole, so that the non-deactivated iron-based catalyst can also burn at a lower temperature, thereby avoiding spontaneous combustion during manual wax removal and causing casualties. After cooling the Fischer-Tropsch synthesis reactor 1 through the top manhole and introducing air through the bottom manhole, the temperature at the top of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling discharged from the top manhole, the composition of the gas to be exhausted after cooling and the CO content therein are detected, so as to accurately determine whether to perform manual wax cleaning. The above-mentioned treatment method of the present invention can destroy the structure of the remaining iron-based catalyst that has not been inactivated multiple times, thereby greatly reducing the risk of casualties caused by manual wax cleaning by personnel during the rescue process.
[0045] In one embodiment of the present application, when the concentration of combustible gas in the first product is <5LEL%, the compressor is suspended for 2 to 3 hours and then static cooking is performed; and / or the dynamic cooking time is 12 to 16 hours, and / or the dynamic cooking temperature is 150 to 160°C, and / or the static cooking time is 14 to 18 hours, and / or the static cooking temperature is 150 to 180°C; and / or the amount of desalted water introduced is 10 to 20 tons / hour.
[0046] Preferably, when the concentration of combustible gas in the first product is <5LEL%, it is qualified. After pausing the compressor for the above time, static cooking is performed again, which helps to relieve the system pressure after pausing the compressor, and all the blind plates connecting the Fischer-Tropsch synthesis reactor 1 to the torch are blinded. After confirming that the Fischer-Tropsch synthesis reactor 1 is isolated from the torch, static cooking is performed to help prevent the flare gas from flowing back as much as possible. It is preferred to control the temperature and time of dynamic cooking and static cooking within the above range, which helps to increase the content of free water, thereby further enhancing the destructiveness to the iron-based catalyst. It is preferred to control the amount of desalted water to be within the above range, which helps to fully rinse the iron-based catalyst attached to the cyclone separator 4, and plays a role in cooling the Fischer-Tropsch synthesis reactor 1, so that the desalted water vaporizes and destroys the activity of the iron-based catalyst again, and helps to further improve the degree of damage to the iron-based catalyst structure. The amount of desalted water preferably introduced is 10 tons / hour, preferably by opening the drainage port at the bottom of the Fischer-Tropsch synthesis reactor 1 to guide the observation, if the guide does not contain water, the amount of desalted water introduced is adjusted to 15 tons to 20 tons / hour.
[0047] In one embodiment of the present application, after the desalted water is passed for flushing, the temperature at the top of the Fischer-Tropsch synthesis reactor 1 is tested. When the temperature at the top of the Fischer-Tropsch synthesis reactor 1 is ≥70°C, the opening angle of the top manhole is opened to 90°, and water is passed into the Fischer-Tropsch synthesis reactor 1 through the top manhole while the second nitrogen is passed for cooling for 20 to 25 minutes. Then, the second nitrogen is stopped and the opening angle of the bottom manhole is opened to 10 to 15°. The top temperature of the Fischer-Tropsch synthesis reactor 1, the gas state of the gas to be exhausted after cooling, the composition of the gas to be exhausted after cooling, and the CO content therein are measured. First test; the qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is ≤40°C, and the gas to be discharged after cooling is in a water vapor state and does not contain flue gas, and the CO content in the gas to be discharged after cooling is <25ppm; when the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is ≥50°C, the gas to be discharged after cooling is in a water vapor state and contains flue gas, and the CO content in the gas to be discharged after cooling is ≥25ppm, water is introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes every 30 minutes to cool it down and continue for 2 hours until the test result is qualified; then the opening angle of the bottom manhole is adjusted to The opening angle is increased by 15 to 20 degrees each time until the opening angle is 90 degrees. If the test result is qualified, the Fischer-Tropsch synthesis reactor 1 is entered through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole, before each time the bottom manhole is opened to a new angle, ensure that the test result is qualified. Otherwise, water is introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes every 30 minutes to cool it down and continue for 2 hours until the test result is qualified. When the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is less than 50°C, and the gas to be discharged after cooling is water vapor state, excluding flue gas, when the CO content in the exhaust gas after cooling is <25ppm, the opening angle of the bottom manhole is increased by 15 to 20° each time until the opening angle is 90°. If the test result is qualified, enter the Fischer-Tropsch synthesis reactor 1 through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, each time before the bottom manhole opens a new angle, ensure that the test result is qualified, otherwise, water is introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes for cooling every 30 minutes and continued for 2 hours until the test result is qualified.
[0048] By controlling the opening angles of the top manhole and the bottom manhole to adjust the amount of water and nitrogen introduced, it is helpful to cool down the Fischer-Tropsch synthesis reactor 1 and detect the temperature at the top of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling and discharged from the top manhole, the composition of the gas to be exhausted after cooling and whether the CO content therein is in a qualified state, thereby helping to further accurately determine whether manual wax cleaning can be performed and effectively clean the wax accumulated inside the Fischer-Tropsch synthesis reactor 1, while ensuring personnel safety. Among them, when the opening angle of the bottom manhole is 90° for the last detection, continuous detection for 2 hours is required, during which detection is performed every 10 minutes or 30 minutes, and the CO content is less than 25ppm, thereby ensuring the safety of the manual wax cleaning process.
[0049] The beneficial effects of the present application will be further illustrated below in conjunction with embodiments.
[0050] Example 1
[0051] Use Figure 1 The Fischer-Tropsch synthesis reaction device shown in the figure performs oxidation deactivation on the iron-based catalyst in the Fischer-Tropsch synthesis reaction product system to facilitate manual wax removal. Specifically, the first steam boiling line A-1 connected to the pipeline of the nitrogen pipeline B-2 at the bottom of the Fischer-Tropsch synthesis reactor 1 is mixed with the first steam and the first nitrogen at 110°C respectively delivered from the compressor through the circulating nitrogen pipeline B-1 before entering the Fischer-Tropsch synthesis reactor 1 to obtain a mixed gas including the first steam and the first nitrogen. The mixed gas passes through the distributor and enters the Fischer-Tropsch synthesis reactor 1. At the same time, the bottom steam boiling line A-2 connected to the pipeline of the bottom catalyst feeding port C-1 inputs the second steam and enters the Fischer-Tropsch synthesis reactor 1 for dynamic boiling for 16 hours, and the gas in the Fischer-Tropsch synthesis reactor 1 is replaced by the first nitrogen and the structure of the iron-based catalyst is destroyed by the first steam and the second steam to obtain the first product. Among them, the nominal diameter of the first steam boiling line A-1 is 80mm, the pressure of the first steam is 1.0MPa, the pressure of the second steam is 1.0MPa, and the temperature of dynamic boiling is 150°C.
[0052] After the dynamic cooking is completed, the combustible gas in the first product is discharged into the flare system connected to the Fischer-Tropsch synthesis reactor 1. After the combustible gas concentration in the first product after the combustible gas is removed in the Fischer-Tropsch synthesis reactor 1 is less than 5LEL%, the compressor is suspended for 2 hours and the system is depressurized, all blind plates connected to the flare system are reversed, and the desalted water pipeline on the outer wall of the top of the Fischer-Tropsch synthesis reactor 1 is connected. The upper steam cooking pipeline A-3, the middle steam cooking pipeline A-4, the lower steam cooking pipeline A-5 and the bottom steam cooking line A-2 connected to the pipelines of the first steam cooking line A-1, the upper catalyst discharge port C-2, the middle catalyst discharge port C-3 and the lower catalyst discharge port C-4 are respectively connected to enter the Fischer-Tropsch synthesis reactor 1 for static cooking for 14 hours to obtain heavy products including wax and iron-based catalysts and gases to be discharged. At the same time, during the static cooking, a small amount of cold second nitrogen is introduced through the nitrogen pipeline B-2 to maintain the pressure in the Fischer-Tropsch synthesis reactor 1 at 0.1MPa.
[0053] The Fischer-Tropsch synthesis reactor 1 is provided with heat exchange tubes 2, which include upper heat exchange tubes 21 and lower heat exchange tubes 22. The steam drum 3 includes an upper steam drum 31 and a lower steam drum 32, which are connected to the upper heat exchange tubes 21 and the lower heat exchange tubes 22, respectively. During the static cooking process, by adjusting the steam flow rate of the 5.4MPa upper drum steam pipeline A-6 and the 5.4MPa lower drum steam pipeline A-7 connected to the upper drum 31 and the lower drum 32 in the drum 3, the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1 is controlled at 150°C, and the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 is controlled at 200°C, the wax and iron-based catalyst attached to the upper heat exchange tube 21 are melted to obtain heavy products including wax and iron-based catalysts, and the heavy products fall to the bottom of the Fischer-Tropsch synthesis reactor 1 by gravity. After the static cooking is completed, the wax and the deactivated iron-based catalyst are evaporated and dehydrated through the waste catalyst recovery tank with a stirring device at the bottom, and then pressure-sent to the pressure tank 5 through the lower catalyst discharge port C-4. The static cooking temperature is 150°C.
[0054] 10 cyclone separators are arranged near the top of the Fischer-Tropsch synthesis reactor 1 and are arranged inside the Fischer-Tropsch synthesis reactor 1. Each cyclone separator is arranged in a horizontal ring shape, and there is a horizontal distance of 1m between each cyclone separator and the inner wall of the Fischer-Tropsch synthesis reactor 1. The pressure of the Fischer-Tropsch synthesis reactor 1 is unloaded to normal pressure, and the desalted water pipelines at the first desalted water valve D-1, the second desalted water valve D-2 and the third desalted water valve D-3 are opened to introduce desalted water into the Fischer-Tropsch synthesis reactor 1 to flush the iron-based catalyst on the top of the cyclone separator 4, and to cool the Fischer-Tropsch synthesis reactor 1. At the same time, the desalted water is vaporized after entering the Fischer-Tropsch synthesis reactor 1, and the water vapor destroys the remaining iron-based catalyst structure and quickly deactivates it. The amount of desalted water introduced is 10 tons / hour.
[0055] After the desalted water was flushed, the temperature at the top of the Fischer-Tropsch synthesis reactor 1 was tested to be 100°C. The opening angle of the top manhole was opened to 90°, and water was passed into the manhole to cool it down for 20 minutes. At the same time, 8000 Nm 3 / h of the second nitrogen is cooled, and then the opening angle of the bottom manhole is opened to 15°. After the gas to be exhausted after cooling is obtained, the top temperature of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling, the composition of the gas to be exhausted after cooling, and the content of CO therein are first detected. The qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is ≤40°C, and the gas to be exhausted after cooling is in a water vapor state and does not contain flue gas, and the content of CO in the gas to be exhausted after cooling is <25ppm. If any one of the items is not met, it is unqualified.
[0056] The result of the first test was that the top temperature of the Fischer-Tropsch synthesis reactor 1 was 60°C, the gas to be discharged after cooling was in a water vapor state and contained flue gas, and the CO content in the gas to be discharged after cooling was 28 ppm. Water was introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes every 30 minutes for cooling and continued for 2 hours until the second test result was qualified.
[0057] Then, the opening angle of the bottom manhole is opened to 35° for the third test, and the third test result is qualified. The opening angle of the bottom manhole is further opened to 55° for the fourth test, and the fourth test result is qualified. The opening angle of the bottom manhole is further opened to 75° for the fifth test, and the fifth test result is qualified. The opening angle of the bottom manhole is further opened to 90° for the sixth test, and the sixth test result is qualified. Each test result is in a qualified state, and the Fischer-Tropsch synthesis reactor 1 is entered through the top manhole and the bottom manhole for manual wax removal. Among them, in the sixth test, that is, the last test, continuous detection is carried out for 2h, during which detection is performed once every 10min, and the CO content is less than 25ppm.
[0058] Example 2
[0059] Use Figure 1The Fischer-Tropsch synthesis reaction device shown in the figure performs oxidation deactivation on the iron-based catalyst in the Fischer-Tropsch synthesis reaction product system to facilitate manual wax removal. Specifically, the first steam boiling line A-1 connected to the pipeline of the nitrogen pipeline B-2 at the bottom of the Fischer-Tropsch synthesis reactor 1 is mixed with the first steam and the first nitrogen at 120°C respectively delivered from the compressor through the circulating nitrogen pipeline B-1 before entering the Fischer-Tropsch synthesis reactor 1 to obtain a mixed gas including the first steam and the first nitrogen. The mixed gas passes through the distributor and enters the Fischer-Tropsch synthesis reactor 1. At the same time, the bottom steam boiling line A-2 connected to the pipeline of the bottom catalyst feeding port C-1 inputs the second steam into the Fischer-Tropsch synthesis reactor 1 for dynamic boiling for 12 hours, and the gas in the Fischer-Tropsch synthesis reactor 1 is replaced by the first nitrogen and the structure of the iron-based catalyst is destroyed by the first steam and the second steam to obtain the first product. Among them, the nominal diameter of the first steam boiling line A-1 is 80mm, the pressure of the first steam is 1.0MPa, the pressure of the second steam is 1.0MPa, and the temperature of dynamic boiling is 160°C.
[0060] After the dynamic cooking is completed, the combustible gas in the first product is discharged into the flare system connected to the Fischer-Tropsch synthesis reactor 1. After the combustible gas concentration in the first product after the combustible gas is removed in the Fischer-Tropsch synthesis reactor 1 is less than 5LEL%, the compressor is suspended for 3 hours and then the system is depressurized, all blind plates connected to the flare system are reversed, and the desalted water pipeline on the outer side wall of the top of the Fischer-Tropsch synthesis reactor 1 is connected. The upper steam cooking pipeline A-3, the middle steam cooking pipeline A-4, the lower steam cooking pipeline A-5 and the bottom steam cooking line A-2 connected to the pipelines of the first steam cooking line A-1, the upper catalyst discharge port C-2, the middle catalyst discharge port C-3 and the lower catalyst discharge port C-4 are respectively input into the Fischer-Tropsch synthesis reactor 1 for static cooking for 14 hours to obtain heavy products including wax and iron-based catalysts and gases to be discharged. At the same time, during the static cooking, a small amount of cold second nitrogen is introduced through the nitrogen pipeline B-2 to maintain the pressure in the Fischer-Tropsch synthesis reactor 1 at 0.15MPa.
[0061] The Fischer-Tropsch synthesis reactor 1 is provided with heat exchange tubes 2, which include upper heat exchange tubes 21 and lower heat exchange tubes 22. The steam drum 3 includes an upper steam drum 31 and a lower steam drum 32, which are connected to the upper heat exchange tubes 21 and the lower heat exchange tubes 22, respectively. During the static cooking process, by adjusting the steam flow rate of the 5.4MPa upper drum steam pipeline A-6 and the 5.4MPa lower drum steam pipeline A-7 connected to the upper drum 31 and the lower drum 32 in the drum 3, the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1 is controlled at 140°C, and the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 is controlled at 180°C, the wax and iron-based catalyst attached to the upper heat exchange tubes 21 are melted to obtain heavy products including wax and iron-based catalysts, and the heavy products fall to the bottom of the Fischer-Tropsch synthesis reactor 1 by gravity. After the static cooking is completed, the wax and the deactivated iron-based catalyst are evaporated and dehydrated through the waste catalyst recovery tank with a stirring device at the bottom, and then pressure-sent to the pressure tank 5 through the lower catalyst discharge port C-4. The temperature of the static cooking is 180°C.
[0062] 10 cyclone separators are arranged near the top of the Fischer-Tropsch synthesis reactor 1 and in the Fischer-Tropsch synthesis reactor 1. Each cyclone separator is arranged in a horizontal ring shape, and there is a horizontal distance of 1m between each cyclone separator and the inner wall of the Fischer-Tropsch synthesis reactor 1. The pressure of the Fischer-Tropsch synthesis reactor 1 is unloaded to normal pressure, and the desalted water pipelines at the first desalted water valve D-1, the second desalted water valve D-2 and the third desalted water valve D-3 are opened to introduce desalted water into the Fischer-Tropsch synthesis reactor 1 to flush the iron-based catalyst on the top of the cyclone separator 4, and to cool the Fischer-Tropsch synthesis reactor 1. At the same time, the desalted water is vaporized after entering the Fischer-Tropsch synthesis reactor 1, and the water vapor destroys the remaining iron-based catalyst structure and quickly deactivates it. Among them, the amount of desalted water introduced is 10 tons / hour. By opening the drainage port at the bottom of the reactor to guide the dripping and observe, the dripping place does not contain water, and the amount of desalted water is adjusted to 20 tons / hour.
[0063] After the desalted water was flushed, the temperature at the top of the Fischer-Tropsch synthesis reactor 1 was tested to be 80°C. The opening angle of the top manhole was opened to 90°, and water was passed into the manhole to cool it down for 25 minutes. At the same time, 8000 Nm of nitrogen was passed through the nitrogen pipeline B-2. 3 / h of the second nitrogen is cooled, and then the opening angle of the bottom manhole is opened to 15°. After the gas to be exhausted after cooling is obtained, the top temperature of the Fischer-Tropsch synthesis reactor 1 and the gas state of the gas to be exhausted after cooling, the composition of the gas to be exhausted after cooling, and the content of CO therein are first detected. The qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor 1 is ≤40°C, and the gas to be exhausted after cooling is in a water vapor state and does not contain flue gas, and the content of CO in the gas to be exhausted after cooling is <25ppm. If any one of the items is not met, it is unqualified.
[0064] The result of the first test was that the top temperature of the Fischer-Tropsch synthesis reactor 1 was 40°C, the gas to be discharged after cooling was in a water vapor state and did not contain flue gas, and the CO content in the gas to be discharged after cooling was 23ppm, the opening angle of the bottom manhole was opened to 35°, and the second test result was qualified. The opening angle of the bottom manhole was further opened to 55° for the third test, and the result of the third test was that the gas to be discharged after cooling was in a water vapor state and contained flue gas, and the CO content in the gas to be discharged after cooling was 27ppm. Water was introduced into the Fischer-Tropsch synthesis reactor 1 for 10 minutes every 30 minutes for cooling and continued for 2 hours until the third test result was qualified.
[0065] The opening angle of the bottom manhole is further opened to 75° for the fourth test, and the fourth test result is qualified. The opening angle of the bottom manhole is further opened to 90° for the fifth test, and the fifth test result is qualified. Each test result is qualified, and the Fischer-Tropsch synthesis reactor 1 is entered through the top manhole and the bottom manhole for manual wax removal. Among them, in the fifth test, which is the last test, continuous testing is carried out for 2 hours, during which the test is carried out every 30 minutes, and the CO content is less than 25ppm.
[0066] Comparative Example 1
[0067] The difference from Example 1 is that desalted water is not used to clean the cyclone separator 4. When the opening angle of the bottom manhole is finally opened to 90°, the top temperature of the Fischer-Tropsch synthesis reactor 1 is detected to be 50°C and the gas to be discharged after cooling is in a water vapor state, containing flue gas, and the CO content in the gas to be discharged after cooling is 32 ppm.
[0068] Comparative Example 2
[0069] The difference from Example 1 is that the temperature of the upper section and the temperature of the lower section of the Fischer-Tropsch synthesis reactor 1 are the same, both of which are 220°C. Finally, the top temperature of the Fischer-Tropsch synthesis reactor 1 and the composition of the mixed gas to be tested, the CO content and the gas state are detected. Finally, when the opening angle of the bottom manhole is further opened to 90°, the top temperature of the Fischer-Tropsch synthesis reactor 1 is detected to be 60°C and the gas to be discharged after cooling is in a water vapor state, containing flue gas, and the CO content in the gas to be discharged after cooling is 35ppm.
[0070] Test method:
[0071] The top temperature of the Fischer-Tropsch synthesis reactor is measured by a remote thermometer, the composition of the gas to be exhausted after cooling is detected by a portable four-in-one gas detector, the content of CO in the gas to be exhausted after cooling is detected by a portable carbon monoxide detector, and the gas state is determined by observing whether there is water mist in the gas to be exhausted after cooling.
[0072] Among them, in Comparative Example 1, since desalted water was not used to clean the cyclone separator 4, a large amount of iron-based catalyst remained on the cyclone separator 4, resulting in spontaneous combustion after the manhole was opened. In Comparative Example 2, since the temperature of the upper section of the Fischer-Tropsch synthesis reactor 1 was the same as the temperature of the lower section, a large amount of wax and iron-based catalyst remained on the upper heat exchange tubes 21, resulting in spontaneous combustion after the manhole was opened. None of the above examples experienced the above spontaneous combustion.
[0073] From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:
[0074] The present application provides a Fischer-Tropsch synthesis reaction device for the scenario of oxidative deactivation of iron-based catalysts in the Fischer-Tropsch synthesis reaction. By adding static cooking on the basis of dynamic cooking in the Fischer-Tropsch synthesis reactor, the iron-based catalyst and wax attached to the upper heat exchange tubes in the Fischer-Tropsch synthesis reactor can be dropped to the bottom of the Fischer-Tropsch synthesis reactor under the action of gravity and pressed out, thereby reducing the amount of manual wax removal. At the same time, static cooking has a higher degree of damage to the iron-based catalyst. The iron-based catalyst on the cyclone separator in the Fischer-Tropsch synthesis reactor is rinsed with desalted water, and the Fischer-Tropsch synthesis reactor can also be cooled, so that the desalted water vaporizes during the falling process to form water mist and contacts the iron-based catalyst on the top of the cyclone separator, and the activity of the iron-based catalyst remaining on the top of the cyclone separator is destroyed again, and the degree of destruction is higher. Air is introduced through the bottom manhole, so that the non-deactivated iron-based catalyst can also burn at a lower temperature, thereby avoiding spontaneous combustion during manual wax removal and causing casualties. After cooling the Fischer-Tropsch synthesis reactor through the top manhole and introducing air through the bottom manhole, the temperature at the top of the Fischer-Tropsch synthesis reactor and the gas state of the gas to be exhausted after cooling discharged from the top manhole, the composition of the gas to be exhausted after cooling and the CO content therein are detected, so as to accurately judge whether manual wax removal can be performed. The Fischer-Tropsch synthesis reaction device of the present invention can achieve multiple destruction of the structure of the remaining iron-based catalyst that has not been deactivated, and can greatly reduce the risk of casualties of personnel performing manual wax removal during the rescue process.
[0075] The above are only embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. A Fischer-Tropsch synthesis reaction device, characterized in that: The Fischer-Tropsch synthesis reaction device comprises: A Fischer-Tropsch synthesis reactor (1), wherein the Fischer-Tropsch synthesis reactor (1) provides a reaction site for a Fischer-Tropsch synthesis reaction product system including an iron-based catalyst and wax; the Fischer-Tropsch synthesis reactor (1) is used to perform a first oxidation deactivation on the iron-based catalyst by dynamic cooking to obtain a first product, and to perform a second oxidation deactivation on the iron-based catalyst in the first product by static cooking to obtain a heavy product including wax and the iron-based catalyst and a gas to be discharged; The Fischer-Tropsch synthesis reactor (1) is provided with a heat exchange tube (2), and the heat exchange tube (2) comprises an upper heat exchange tube (21) and a lower heat exchange tube (22); the heat exchange tube (2) is used to control the temperature in the Fischer-Tropsch synthesis reactor (1); A steam drum (3), wherein the steam drum (3) is arranged outside the Fischer-Tropsch synthesis reactor (1), and the steam drum (3) comprises an upper steam drum (31) and a lower steam drum (32), wherein the upper steam drum (31) is connected to the upper heat exchange tube (21), and the lower steam drum (32) is connected to the lower heat exchange tube (22), wherein the upper steam drum (31) is used to control the temperature of the upper section of the Fischer-Tropsch synthesis reactor (1), and the lower steam drum (32) is used to control the temperature of the lower section of the Fischer-Tropsch synthesis reactor (1); the steam drum (3) is used to heat and melt the wax and the iron-based catalyst on the upper heat exchange tube (21) during the static cooking to obtain the heavy product; the temperature of the upper section of the Fischer-Tropsch synthesis reactor (1) is higher than the temperature of the lower section of the Fischer-Tropsch synthesis reactor (1); A plurality of cyclone separators (4), each of the cyclone separators (4) being close to the top of the Fischer-Tropsch synthesis reactor (1) and arranged inside the Fischer-Tropsch synthesis reactor (1), the plurality of cyclone separators (4) being arranged in a horizontal ring shape, and each of the cyclone separators (4) having a certain horizontal distance from the inner side wall of the Fischer-Tropsch synthesis reactor (1); The side wall of the top of the Fischer-Tropsch synthesis reactor (1) has a plurality of desalted water inlets, each of which is used to introduce desalted water to flush the iron-based catalyst on the cyclone separator (4) to destroy and deactivate the iron-based catalyst; The Fischer-Tropsch synthesis reactor (1) further comprises a top manhole and a bottom manhole, wherein the bottom manhole is used to introduce air into the Fischer-Tropsch synthesis reactor (1) and burn the undeactivated iron-based catalyst, and the top manhole is used to introduce water into the Fischer-Tropsch synthesis reactor (1) to cool the gas to be discharged, thereby obtaining the cooled gas to be discharged; The top temperature of the Fischer-Tropsch synthesis reactor (1), the gas state of the gas to be exhausted after the temperature is reduced, the composition of the gas to be exhausted after the temperature is reduced, and the CO content therein are detected to determine whether to perform artificial wax removal.
2. The Fischer-Tropsch synthesis reaction device according to claim 1, characterized in that: The bottom of the Fischer-Tropsch synthesis reactor (1) is also provided with a nitrogen pipeline and a circulating nitrogen pipeline; the nitrogen pipeline is connected to a first steam boiling line; The bottom of the Fischer-Tropsch synthesis reactor (1) is also provided with a bottom catalyst feeding port, and the pipeline of the bottom catalyst feeding port is connected to a bottom steam boiling line; The first steam cooking line is used to transport the first steam into the Fischer-Tropsch synthesis reactor (1); the circulating nitrogen pipeline is used to transport the first nitrogen into the Fischer-Tropsch synthesis reactor (1); the bottom steam cooking line is used to transport the second steam into the Fischer-Tropsch synthesis reactor (1); the first steam is mixed with the first nitrogen and then with the second steam for the dynamic cooking; Preferably, the first nitrogen is used to replace the gas in the Fischer-Tropsch synthesis reactor (1); the first steam and the second steam are used to perform the first oxidation deactivation on the iron-based catalyst; Preferably, the nominal diameter of the first steam cooking line is 80 mm, and / or the pressure of the first steam is 1.0 MPa, and / or the pressure of the second steam is 1.0 MPa, and / or the temperature of the first nitrogen is 110-120° C., and / or the nominal diameter of the bottom steam cooking line is 40 mm.
3. The Fischer-Tropsch synthesis reaction device according to claim 2, characterized in that: An upper catalyst discharge port, a middle catalyst discharge port and a lower catalyst discharge port are sequentially arranged on the outer wall of the Fischer-Tropsch synthesis reactor (1) in the axial direction of the Fischer-Tropsch synthesis reactor (1), and the pipelines of the upper catalyst discharge port, the middle catalyst discharge port and the lower catalyst discharge port are respectively connected with an upper steam cooking pipeline, a middle steam cooking pipeline and a lower steam cooking pipeline, and the upper steam cooking pipeline, the middle steam cooking pipeline, the lower steam cooking pipeline and the bottom steam cooking line are used to transport the third steam into the Fischer-Tropsch synthesis reactor (1) for the static cooking; And / or, when the static cooking is carried out, the pressure in the Fischer-Tropsch synthesis reactor (1) is 0.1-0.15 MPa, and the nominal diameters of the upper steam cooking line, the middle steam cooking line and the lower steam cooking line are each independently 40 mm.
4. The Fischer-Tropsch synthesis reaction device according to any one of claims 1 to 3, characterized in that: The inlet pipelines of the upper steam drum (31) and the lower steam drum (32) are respectively connected with an upper steam drum steam pipeline and a lower steam drum steam pipeline; the pressures of the steam transported by the upper steam drum steam pipeline and the lower steam drum steam pipeline are independently 5.4 MPa; the temperature of the lower section of the Fischer-Tropsch synthesis reactor (1) is 140-150°C, and the temperature of the upper section of the Fischer-Tropsch synthesis reactor (1) is 180-200°C.
5. The Fischer-Tropsch synthesis reaction device according to any one of claims 1 to 4, characterized in that: The Fischer-Tropsch synthesis reaction device further comprises a compressor, which is in communication with the circulating nitrogen pipeline and is used to circulate the first nitrogen in the dynamic cooking process; And / or, the nitrogen pipeline is used to provide a second nitrogen gas to the Fischer-Tropsch synthesis reactor (1) for cooling, and the feed amount of the second nitrogen gas is 8000-9000 Nm 3 / h; And / or, the Fischer-Tropsch synthesis reaction device further comprises a pressure tank connected to the Fischer-Tropsch synthesis reactor (1), and the heavy product is pressure-fed into the pressure tank through the lower catalyst discharge port.
6. The Fischer-Tropsch synthesis reaction device according to any one of claims 1 to 5, characterized in that: The combustible gas in the first product is discharged into a flare system connected to the Fischer-Tropsch synthesis reactor (1).
7. The Fischer-Tropsch synthesis reaction device according to any one of claims 1 to 6, characterized in that: The opening angles of the top manhole and the bottom manhole are independently 10 to 90°; and / or, after the desalted water is introduced for flushing, the temperature of the top of the Fischer-Tropsch synthesis reactor (1) is tested, and when the temperature of the top of the Fischer-Tropsch synthesis reactor (1) is ≥70°C, the opening angle of the top manhole is opened to 90°, and the water is introduced into the Fischer-Tropsch synthesis reactor (1) through the top manhole while the second nitrogen is introduced to cool the reactor for 20 to 25 minutes, and then the introduction of the second nitrogen is stopped and the opening angle of the bottom manhole is opened to 10 to 15°, and a first detection is performed on the top temperature of the Fischer-Tropsch synthesis reactor (1), the gas state of the gas to be exhausted after the cooling, the composition of the gas to be exhausted after the cooling, and the CO content therein; The qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor (1) is ≤40°C, and the gas to be discharged after cooling is in a water vapor state and does not contain flue gas, and the content of CO in the gas to be discharged after cooling is <25ppm; When the result of the first detection is that the top temperature of the Fischer-Tropsch synthesis reactor (1) is ≥50°C, the gas to be discharged after the cooling is in a water vapor state and contains flue gas, and the content of CO in the gas to be discharged after the cooling is ≥25ppm, the water is introduced into the Fischer-Tropsch synthesis reactor (1) for 10 minutes every 30 minutes to cool the reactor for 2 hours until the detection result is qualified; Subsequently, the opening angle of the bottom manhole is increased by 15 to 20 degrees each time until the opening angle reaches 90 degrees. If the test result is qualified, the Fischer-Tropsch synthesis reactor (1) is entered through the top manhole and the bottom manhole to perform the manual wax removal. In the process of opening the bottom manhole, before each time the bottom manhole is opened to a new angle, it is ensured that the test result is qualified. Otherwise, the water is introduced into the Fischer-Tropsch synthesis reactor (1) for 10 minutes at intervals of 30 minutes for cooling, and the cooling is continued for 2 hours until the test result is qualified. When the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor (1) is less than 50°C, and the gas to be exhausted after cooling is in a water vapor state and does not contain flue gas, and the CO content in the gas to be exhausted after cooling is less than 25ppm, the opening angle of the bottom manhole is increased by 15 to 20° each time until the opening angle is 90°, and the test result is qualified, then the Fischer-Tropsch synthesis reactor (1) is entered through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, each time before the bottom manhole is opened to a new angle, ensure that the test result is qualified, otherwise the water is introduced into the Fischer-Tropsch synthesis reactor (1) for 10 minutes every 30 minutes for cooling and the cooling is continued for 2 hours until the test result is qualified.
8. A method for treating oxidative deactivation of an iron-based catalyst using the Fischer-Tropsch synthesis reaction device according to any one of claims 1 to 7, characterized in that: The processing method comprises: In a Fischer-Tropsch synthesis reactor (1), the iron-based catalyst in a Fischer-Tropsch synthesis reaction product system comprising an iron-based catalyst and wax is subjected to a first oxidation deactivation by dynamic cooking to obtain a first product; the iron-based catalyst in the first product is subjected to a second oxidation deactivation by static cooking to obtain a heavy product comprising wax and the iron-based catalyst and a gas to be discharged; During the static cooking, the wax and the iron-based catalyst on the upper heat exchange tube (21) are heated and melted to obtain the heavy product; the temperature of the upper section of the Fischer-Tropsch synthesis reactor (1) is higher than the temperature of the lower section of the Fischer-Tropsch synthesis reactor (1); flushing the iron-based catalyst on the cyclone separator (4) with desalted water to destroy and deactivate the iron-based catalyst; Air is introduced into the Fischer-Tropsch synthesis reactor (1) through the bottom manhole to burn the undeactivated iron-based catalyst, and water is introduced into the Fischer-Tropsch synthesis reactor (1) through the top manhole to cool the gas to be discharged, thereby obtaining the cooled gas to be discharged; Whether to perform artificial wax removal is determined by detecting the top temperature of the Fischer-Tropsch synthesis reactor (1), the gas state of the gas to be exhausted after the temperature is reduced, the composition of the gas to be exhausted after the temperature is reduced, and the CO content therein.
9. The processing method according to claim 8, characterized in that: When the concentration of the combustible gas in the first product is less than 5LEL%, the compressor is stopped for 2 to 3 hours before the static cooking is performed; and / or, the dynamic cooking time is 12 to 16 hours, the dynamic cooking temperature is 150 to 160° C., and / or, the static cooking time is 14 to 18 hours, and / or, the static cooking temperature is 150 to 180° C.; And / or, the amount of desalted water introduced is 10 to 20 tons / hour.
10. The processing method according to claim 8 or 9, characterized in that: After the desalted water is introduced for flushing, the temperature of the top of the Fischer-Tropsch synthesis reactor (1) is tested. When the temperature of the top of the Fischer-Tropsch synthesis reactor (1) is ≥70°C, the opening angle of the top manhole is opened to 90°, and the water is introduced into the Fischer-Tropsch synthesis reactor (1) through the top manhole while the second nitrogen is introduced to cool the reactor for 20 to 25 minutes. Then, the introduction of the second nitrogen is stopped and the opening angle of the bottom manhole is opened to 10 to 15°. The top temperature of the Fischer-Tropsch synthesis reactor (1), the gas state of the gas to be exhausted after the cooling, the composition of the gas to be exhausted after the cooling, and the CO content therein are first detected. The qualified state of the test result is that the top temperature of the Fischer-Tropsch synthesis reactor (1) is ≤40°C, and the gas to be discharged after cooling is in a water vapor state and does not contain flue gas, and the content of CO in the gas to be discharged after cooling is <25ppm; When the result of the first detection is that the top temperature of the Fischer-Tropsch synthesis reactor (1) is ≥50°C, the gas to be discharged after the cooling is in a water vapor state and contains flue gas, and the content of CO in the gas to be discharged after the cooling is ≥25ppm, the water is introduced into the Fischer-Tropsch synthesis reactor (1) for 10 minutes every 30 minutes to cool the reactor for 2 hours until the detection result is qualified; Subsequently, the opening angle of the bottom manhole is increased by 15 to 20 degrees each time until the opening angle reaches 90 degrees. If the test result is qualified, the Fischer-Tropsch synthesis reactor (1) is entered through the top manhole and the bottom manhole to perform the manual wax removal. In the process of opening the bottom manhole, before each time the bottom manhole is opened to a new angle, it is ensured that the test result is qualified. Otherwise, the water is introduced into the Fischer-Tropsch synthesis reactor (1) for 10 minutes at intervals of 30 minutes for cooling, and the cooling is continued for 2 hours until the test result is qualified. When the result of the first test is that the top temperature of the Fischer-Tropsch synthesis reactor (1) is less than 50°C, and the gas to be exhausted after cooling is in a water vapor state and does not contain flue gas, and the CO content in the gas to be exhausted after cooling is less than 25ppm, the opening angle of the bottom manhole is increased by 15 to 20° each time until the opening angle is 90°, and the test result is qualified, then the Fischer-Tropsch synthesis reactor (1) is entered through the top manhole and the bottom manhole for manual wax cleaning; and in the process of opening the bottom manhole angle, each time before the bottom manhole is opened to a new angle, ensure that the test result is qualified, otherwise the water is introduced into the Fischer-Tropsch synthesis reactor (1) for 10 minutes every 30 minutes for cooling and the cooling is continued for 2 hours until the test result is qualified.
Citation Information
Patent Citations
Extraction method of heavy fraction of ft synthetic product from slurry bed reactor
CN101391196A
Regeneration method of microchannel reactor Fischer-Tropsch synthesis catalyst
CN109201074A
Regeneration method of Fischer-Tropsch synthesis catalyst
CN115041194A
Fluidized bed activation system for Fischer-Tropsch synthesis iron-based catalyst
CN117343754A
Fischer-Tropsch synthesis catalyst activation system and interlocking protection control method
CN117504740A