Rapid soaking method for catalysts used in MTBE production

Abstract

The present invention relates to the technical field of catalyst preparation, and in particular to a rapid soaking method for catalysts used in MTBE production, the method comprising: periodically acquiring the actual reflux water level rise rate with a preset initial duration, calculating the water level rise rate change between the actual reflux water level rise rates at any two adjacent acquisition moments, judging whether to start an abnormality inspection mode according to the water level rise rate change, and performing an abnormality inspection on each preparation link according to the abnormality inspection mode, and judging to start an extraction mode based on the fact that each preparation link is qualified. The present invention avoids a large amount of methanol remaining in the catalyst by replacing methanol with carbon four after ether, reduces the unqualified MTBE product caused by methanol accumulation at the bottom of the catalytic distillation tower, and improves the overall operating efficiency of the device; water is pressed out of the catalyst by pressure, thereby improving the soaking replacement efficiency and thus improving the overall production efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of catalyst preparation, in particular to a rapid soaking method for a catalyst used in MTBE production. Background Art

[0002] The etherification reaction system of the MTBE unit usually uses etherified strong acidic large-pore cation exchange resin as a catalyst, which has a high water content (35-55%). Before using the catalyst to catalyze the production of MTBE, it needs to be soaked and dehydrated to reduce the by-products easily generated by the water in the catalyst, which affects the quality and purity of the product. At the same time, because the water entrained in the catalyst cannot be compressed, the pressure drop of the reaction material is large. When the air velocity reaches the upper limit, it has a destructive effect on the equipment.

[0003] The traditional methanol soaking water replacement process uses the fact that methanol and water can dissolve in each other, and the alcohol and water are recovered after the water is precipitated. The methanol remaining in the catalyst bed after soaking with methanol can easily make the alcohol-olefin ratio difficult to control in the initial stage of feed. It takes a long time to adjust the expected effect of the reaction after the start of operation. At the same time, the methanol content in the stripping section of the catalytic distillation tower is high, and excessive methanol is entrained into the main product MTBE and remains unqualified for a long time (MTBE product requires MeOH≯0.5%). Therefore, it is particularly important to solve the two problems of water replacement of acidic large-pore cation exchange resin catalysts and shortening the long quality adjustment cycle of traditional pretreatment processes due to methanol soaking. Summary of the invention

[0004] To this end, the purpose of the present invention is to provide a rapid soaking method for catalysts used in MTBE production, so as to overcome the problem that the current catalyst preparation technology cannot guarantee product quality and production efficiency.

[0005] To achieve the above object, the present invention provides a rapid soaking method for a catalyst used in MTBE production, comprising:

[0006] delivering the initial soaking raw material to the pre-reactor at a preset initial controlled flow rate, and pre-treating the initial soaking raw material in the pre-reactor to obtain the target soaking raw material;

[0007] Performing real-time monitoring on the pretreatment process to obtain pretreatment monitoring results, and determining whether to start the immersion replacement mode according to the pretreatment monitoring results;

[0008] Based on starting the soaking and replacement mode, the target soaking raw material is delivered to the reactor at a target controlled flow rate, the initial production catalyst is soaked and replaced in the reactor according to the target soaking raw material to obtain an intermediate mixture, the soaking and replacement process is monitored in real time to obtain actual monitoring results, and whether the actual reaction process is qualified is determined according to the actual monitoring results;

[0009] Based on the actual reaction process being qualified, the intermediate mixture is subjected to catalytic distillation to form a gaseous mixture;

[0010] Dehydrating and extracting the gaseous mixture in sequence to obtain the actual soaking raw material;

[0011] collecting the actual soaking raw materials to perform a raw material circulation mode;

[0012] In the process of dehydrating the gaseous mixture, the actual reflux water level rising speed is periodically obtained with a preset initial time length, and the water level rising speed change between the actual reflux water level rising speeds at any two adjacent acquisition moments is calculated. According to the water level rising speed change, it is determined whether to start the abnormality inspection mode, and an abnormality inspection is performed on each preparation link according to the abnormality inspection mode. If each preparation link is qualified, it is determined to start the extraction mode;

[0013] Each preparation link includes: a feed introduction link for conveying the target soaking raw material to the reactor, a soaking link for the reactor, and a dehydration link for the reflux tank of the catalytic distillation tower.

[0014] Further, the process of determining whether to start the immersion replacement mode according to the pretreatment monitoring result includes:

[0015] The initial soaking raw material is transported and heated to obtain the target soaking raw material;

[0016] Monitor the conveying process in real time to obtain actual monitoring images;

[0017] Monitor the heating process in real time to obtain the actual temperature;

[0018] Determining whether to start the immersion replacement mode according to the actual monitoring image and the actual temperature;

[0019] Wherein, the pretreatment process includes: the conveying process and the heating process.

[0020] Further, the process of determining whether to start the immersion replacement mode according to the actual monitoring image and the actual temperature includes:

[0021] Based on the actual temperature reaching a preset standard temperature variation range, it is determined that the actual temperature meets the kinetic energy determination condition;

[0022] Obtaining an actual maintenance time during which the actual temperature meets the kinetic energy determination condition, and determining whether the actual temperature meets a single determination condition according to the actual maintenance time;

[0023] Analyzing the actual monitoring image to obtain an actual image monitoring result, and determining that the actual monitoring image meets the single determination condition based on the actual image monitoring result indicating that there is no foam or turbulence;

[0024] Determining whether to start the immersion replacement mode according to the actual temperature and the number of items in the actual monitoring image that meet the single determination condition, and starting the immersion replacement mode based on the number of items being 2;

[0025] Among them, based on the actual maintenance time reaching the preset standard maintenance time, it is determined that the actual temperature meets the single judgment condition; based on the actual maintenance time not reaching the standard maintenance time, it is determined that the actual temperature does not meet the single judgment condition.

[0026] Further, based on the actual image monitoring result indicating the presence of foam or turbulence, it is determined that the actual monitoring image does not meet the single determination condition, and a first adjustment signal is issued;

[0027] adjusting the initial control flow according to the first adjustment signal to obtain the target control flow;

[0028] Based on the actual monitoring image meeting the single determination condition, a first determination signal is issued;

[0029] According to the first determination signal, it is determined that the initial control flow is the target control flow.

[0030] Furthermore, the process of determining whether the actual reaction process is qualified according to the actual monitoring result includes:

[0031] The immersion displacement process is monitored in real time to obtain the actual pressure change rate and the actual temperature change rate;

[0032] Determining whether the actual reaction process meets the first stability condition according to the actual pressure change rate;

[0033] Determining whether the actual reaction process meets the second stability condition according to the actual temperature change rate;

[0034] Based on the fact that the actual reaction process meets both the first stability condition and the second stability condition, it is determined that the actual reaction process is qualified.

[0035] Further, based on the fact that the actual pressure change rate is less than or equal to a preset standard pressure change rate, it is determined that the actual pressure change rate meets the timing determination condition;

[0036] Obtaining a first maintenance time length during which the actual pressure change rate meets the timing determination condition;

[0037] Determining whether the actual reaction process meets the first stability condition according to the first maintenance time;

[0038] Based on the fact that the actual temperature change rate is less than or equal to a preset standard temperature change rate, determining that the actual temperature change rate meets the timing determination condition;

[0039] Obtaining a second maintenance time length during which the actual temperature change rate meets the timing determination condition;

[0040] Whether the actual reaction process meets the second stability condition is determined according to the second maintenance time.

[0041] Furthermore, the process of judging whether to start the abnormality inspection mode according to the change in the water level rising speed includes:

[0042] Determining whether to start the abnormality inspection mode according to the change in the water level rising speed and a preset standard rising speed change;

[0043] Based on the fact that the change in the water level rising speed is less than or equal to the standard change in the water level rising speed, it is determined that the abnormality inspection mode is turned on;

[0044] Based on the fact that the change in the water level rising speed is greater than the standard rising speed change, it is determined that the verification mode is turned on.

[0045] Further, according to the verification mode, the changes of the adjacent water level rising speeds are obtained, and the difference of the changes is calculated according to the changes of the adjacent water level rising speeds;

[0046] Determining whether to adjust the initial duration according to the change amount difference;

[0047] Based on the fact that the variation difference is less than or equal to a preset standard deviation, it is determined that the initial duration is not to be adjusted;

[0048] Based on the fact that the variation difference is greater than the standard deviation, it is determined that a second adjustment signal is sent, and the initial duration is adjusted according to the second adjustment signal to obtain an actual duration.

[0049] Furthermore, the intermediate mixture is transported to a catalytic distillation tower for catalytic distillation, and light components are collected and reflux is established based on a reflux tank of the catalytic distillation tower to dehydrate the gaseous mixture. During the dehydration process, the reflux tank of the catalytic distillation tower is monitored in real time to obtain the actual reflux water level rising rate.

[0050] Furthermore, the process of collecting the actual soaking raw material to perform the raw material circulation mode includes: recycling the actual soaking raw material to obtain the soaking raw material to be recycled, and transporting the soaking raw material to be recycled and reusable as the initial soaking raw material to the pre-reactor;

[0051] Wherein, the actual soaking raw material is the target soaking raw material after the reaction.

[0052] Compared with the prior art, the beneficial effects of the present invention are that the delivery of raw materials is accurately controlled by preset initial control flow and target control flow, thereby ensuring the effectiveness and consistency of the soaking process; real-time monitoring of the pretreatment and soaking replacement processes enables the process to quickly respond to any abnormal situation, thereby improving production efficiency and product quality; the introduction of pretreatment monitoring, soaking replacement mode, and abnormal inspection mode during dehydration enhances the flexibility and controllability of the production process; through real-time monitoring and periodic inspection, problems in production can be discovered and corrected in time to ensure the quality of the final product; the raw material circulation mode is carried out by collecting the actual soaked raw materials after the extraction tower, thereby embodying the principle of sustainable production; not only the waste of raw materials is reduced, but also the environmental footprint of the production process may be reduced.

[0053] Through real-time monitoring and judgment based on actual monitoring images and temperature, the opening of the immersion displacement mode can be controlled more accurately, thereby improving the stability and repeatability of the entire process; by monitoring images to detect the presence of foam or turbulence and adjusting the flow accordingly, it is helpful to reduce or eliminate these undesirable phenomena, thereby avoiding negative impacts on product quality and process efficiency; by monitoring the actual temperature and comparing it with its standard variation range, it can ensure that the raw materials are processed at the optimal temperature, thereby optimizing reaction efficiency and product quality; by precisely controlling temperature and flow, potential safety risks caused by overheating or improper flow are reduced, thereby improving operational safety; by ensuring that the temperature is maintained at the actual required Within the specified range, unnecessary energy consumption is avoided and operating costs are reduced; by precisely controlling the conditions of the immersion displacement process, the quality and consistency of the final product can be improved; adaptive selection and adjustment are made according to the actual preparation accuracy, so that automatic optimization can be achieved according to different operating conditions, thereby improving the flexibility and adaptability of preparation; by precisely controlling the process in the early stages, the generation of unqualified products is reduced, thereby saving resources and reducing waste disposal costs; through automated monitoring and adjustment processes, manual intervention is reduced and production efficiency is improved; by issuing adjustment signals and determining signals, abnormal situations can be responded to in a timely manner, and corresponding adjustment measures can be taken to maintain the continuity and stability of the production process.

[0054] By real-time monitoring of the pressure and temperature change rates and setting standard values, the reaction process can be ensured to be carried out under predetermined stable conditions, thereby improving the quality and consistency of the product; by comparing the actual maintenance time with the standard maintenance time, the reaction conditions can be adjusted in time to optimize the reaction process and reduce unnecessary fluctuations; determining whether the actual reaction process meets the stable conditions helps to promptly discover and correct potential problems, reduce risks in the production process, and avoid the production of unqualified products; by ensuring that the reaction process is carried out under stable conditions, production interruptions and product scrapping due to unstable conditions are reduced, thereby improving production efficiency.

[0055] By monitoring the change in the rate of water level rise, potential abnormalities can be identified in a timely manner and the abnormality inspection mode can be activated to prevent more serious problems from occurring; by promptly activating the abnormality inspection mode, measures can be taken quickly to control or stop operations that may lead to danger, thereby improving the safety of the production process; by introducing the verification mode, further verification can be performed when the change in the rate of water level rise exceeds the standard to avoid misoperation caused by a single data point; by calculating the difference in the changes in adjacent water level rise rates, it can be more accurately determined whether the initial duration needs to be adjusted, thereby achieving more refined process control; by adjusting the initial duration to adapt to actual water level changes, it helps to maintain the stability of the production process and reduce fluctuations.

[0056] Through reflux operation, the light components in the gas mixture can be separated more effectively. By real-time monitoring of the rising speed of the reflux water level in the reflux tank of the catalytic distillation tower, the dehydration process can be better controlled. By deciding whether to turn on the extraction mode based on the rising speed of the reflux water level, it can be ensured that the mode is started only when needed, thereby saving resources and improving efficiency. By recycling the actual soaking raw materials and recycling them as the initial soaking raw materials, the waste of raw materials can be reduced and the production cost can be reduced. The raw material circulation mode allows the production process to be carried out continuously, reducing downtime, and improving the catalyst soaking production efficiency through circulation adjustment. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 This is a flow chart of a rapid soaking method for a catalyst used in MTBE production according to an embodiment of the present invention;

[0058] Figure 2 This is a process flow chart for the post-etherification C4 soaking in the rapid soaking method for the catalyst for MTBE production in an embodiment of the present invention;

[0059] Figure 3 This is a flow chart of determining whether to start the soaking replacement mode in the rapid soaking method for the catalyst for MTBE production according to an embodiment of the present invention;

[0060] Figure 4A flow chart of determining whether the actual reaction process is qualified in a rapid soaking method for a catalyst for MTBE production according to an embodiment of the present invention;

[0061] The figure includes: 1-C4 raw material tank, 2-prereactor, 3-reactor, 4-catalytic distillation tower, 5-catalytic distillation tower reflux tank, 6-extraction tower and 7-post-reaction C4 tank. DETAILED DESCRIPTION

[0062] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0063] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0064] It should be noted that, in the description of the present invention, terms such as "up", "down", "left", "right", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings. This is merely for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.

[0065] See also Figure 1 As shown, the present invention provides a rapid soaking method for a catalyst used in MTBE production, comprising:

[0066] Step S100, delivering the initial soaking raw material to the pre-reactor 2 at a preset initial control flow rate, and pre-treating the initial soaking raw material in the pre-reactor 2 to obtain the target soaking raw material;

[0067] Step S200, real-time monitoring of the pretreatment process to obtain pretreatment monitoring results, and determining whether to start the immersion replacement mode according to the pretreatment monitoring results;

[0068] Step S300, based on starting the soaking and replacement mode, the target soaking raw material is delivered to the reactor 3 at a target controlled flow rate, the initial production catalyst is soaked and replaced in the reactor 3 according to the target soaking raw material to obtain an intermediate mixture, the soaking and replacement process is monitored in real time to obtain an actual monitoring result, and whether the actual reaction process is qualified is determined according to the actual monitoring result;

[0069] Step S400, based on the actual reaction process being qualified, catalytically distilling the intermediate mixture to form a gaseous mixture;

[0070] Step S500, dehydrating and extracting the gaseous mixture in sequence to obtain the actual soaking raw material;

[0071] Step S600, collecting the actual soaking raw materials to perform a raw material circulation mode;

[0072] In the process of dehydrating the gaseous mixture, the actual reflux water level rising speed is periodically obtained with a preset initial time length, and the water level rising speed change between the actual reflux water level rising speeds at any two adjacent acquisition moments is calculated. According to the water level rising speed change, it is determined whether to start the abnormality inspection mode, and an abnormality inspection is performed on each preparation link according to the abnormality inspection mode. If each preparation link is qualified, it is determined to start the extraction mode;

[0073] Each preparation link includes: a feed introduction link for conveying the target soaking raw material to the reactor 3 , a soaking link for the reactor 3 , and a dehydration link for the reflux tank 5 of the catalytic distillation tower.

[0074] In this embodiment, the initial soaking raw material is etherified C4; the initial production catalyst is an acidic large-pore cation exchange resin catalyst; the acidic large-pore cation exchange resin catalyst is soaked in etherified C4 to replace the water in the acidic large-pore cation exchange resin catalyst by extrusion, replacing the original methanol soaking and dissolving pretreatment process; wherein, since the physical properties of etherified C4 and water are quite different, the water can be pressed out of the catalyst by reliable pressure during the soaking process of etherified C4;

[0075] Among them, the target soaking raw material is etherified C4 whose temperature reaches the reaction standard after pretreatment; the specific setting of the initial control flow rate is related to the actual delivery amount of etherified C4 and the actual delivery distance of the MTBE device delivery pipeline; the intermediate mixture is a mixture of etherified C4 and displaced water; the gaseous mixture is an intermediate mixture after heating and distillation; the actual soaking raw material is the etherified C4 to be treated obtained after the water has been separated and extracted;

[0076] The etherified C4 first enters the C4 raw material tank 1, and is led to the pre-reactor 2 for pretreatment by a pump, and then introduced into the reactor 3 equipped with the catalyst for soaking and mixing, and the water is pressed out of the catalyst by increasing the pressure. The intermediate mixture after soaking enters the catalytic distillation tower 4 for distillation process. During distillation, the catalytic distillation tower 4 is heated up, and the steam carrying the etherified C4, that is, the gaseous mixture enters the catalytic distillation tower reflux tank 5, and after dehydration in the catalytic distillation tower reflux tank 5, it enters the extraction tower 6 for extraction of the etherified C4, and the extracted etherified C4 enters the reaction C4 tank 7, and finally returns to the C4 raw material tank 1 through the pump to continue the cycle.

[0077] After the etherification C4 soaking replaced the original methanol soaking, a large amount of methanol remained in the catalyst, which was accumulated at the bottom of the catalytic distillation tower along with the materials, resulting in unqualified MTBE products. It takes 6-7 days for the methanol soaking to completely reduce the methanol content to below 0.5%. At the same time, due to the presence of some moisture in the catalyst, the content of by-product TBA (tert-butyl alcohol) generated by the raw material isobutylene and water in the initial stage of operation is also relatively high. After the methanol soaking, not only a large amount of methanol and unqualified products need to be recovered, but also a large amount of energy is consumed. At the same time, the residual methanol in the catalyst bed is likely to make the alcohol-olefin ratio difficult to control at the initial stage of operation, resulting in too high a methanol content in the MTBE at the bottom of the catalytic distillation tower. The use of etherification C4 soaking can shorten the product qualification adjustment cycle, which is beneficial to the improvement of the operation efficiency of the device. By replacing methanol with etherification C4, a large amount of methanol remained in the catalyst, which reduced the unqualified MTBE products caused by the accumulation of methanol at the bottom of the catalytic distillation tower. It takes 6-7 days for the methanol soaking to complete. The content of TBA (tert-butyl alcohol) in methanol is reduced to below 0.5%, while the use of ether-post-C4 soaking can reach the qualified standard faster, thereby shortening the product qualified adjustment cycle; since there is still some moisture in the catalyst, the by-product TBA (tert-butyl alcohol) content generated by the reaction of raw material isobutylene and water in the initial stage of start-up is relatively high after methanol soaking; ether-post-C4 soaking can reduce this situation and reduce the generation of by-products; a large amount of methanol and unqualified products need to be recovered after methanol soaking, which will consume a lot of energy; the use of ether-post-C4 soaking can reduce this energy consumption and recovery costs; the methanol remaining in the catalyst bed after methanol soaking may make the alcohol-olefin ratio difficult to control, thereby affecting the methanol content in the MTBE at the bottom of the catalytic distillation tower; the use of ether-post-C4 soaking can make it easier to control the alcohol-olefin ratio and improve production stability; by reducing the generation of unqualified products, reducing energy consumption and improving production stability, the overall operating efficiency of the device is improved; the water is pressed out of the catalyst by pressure, the soaking replacement efficiency is improved, thereby improving the overall production efficiency.

[0078] Specifically, the embodiments of the present invention accurately control the delivery of raw materials through preset initial control flow and target control flow, thereby ensuring the effectiveness and consistency of the soaking process; real-time monitoring of the pretreatment and soaking replacement processes enables the process to quickly respond to any abnormal situation, thereby improving production efficiency and product quality; pretreatment monitoring, soaking replacement mode, and abnormal inspection mode during dehydration are introduced to enhance the flexibility and controllability of the production process; through real-time monitoring and periodic inspection, problems in production can be discovered and corrected in a timely manner to ensure the quality of the final product; the raw material circulation mode is carried out by collecting the actual soaked raw materials after the extraction tower, thereby embodying the principle of sustainable production; not only the waste of raw materials is reduced, but also the environmental footprint of the production process may be reduced.

[0079] See also Figure 2 As shown, it is a process flow chart for post-etherification C4 soaking; wherein,

[0080] The C4 raw material tank 1 is used to store the etherified C4 and transport it to the pre-reactor 2 through a pump;

[0081] Pre-reactor 2, which is used to heat the etherified C4 to prepare for the reaction;

[0082] Reactor 3, which is the place where the etherified C4 contacts with the cation exchange resin for soaking and replacement reaction;

[0083] A catalytic distillation tower 4, which is used to perform catalytic reaction and distillation on the intermediate mixture to separate and obtain the gaseous mixture;

[0084] Catalytic distillation tower reflux tank 5, which is used to collect light components and establish reflux to improve separation efficiency;

[0085] An extraction tower 6, which is used to separate the actual soaking raw material from the gaseous mixture;

[0086] After the reaction, the carbon four tank 7 is used to collect the actual soaking raw materials for recycling.

[0087] In this embodiment, when the MTBE device is started, one set of MTBE devices is started first, and another set of devices maintains a sufficient water level in the extraction tower 6. The carbon four after etherification of the MTBE device in operation is collected and fed into the carbon four raw material tank 1. The carbon four is introduced into the reactor 3 equipped with a catalyst by a centrifugal pump, and the pressure is ensured to be stable and a small flow rate is maintained. According to the flow of the production process, the carbon four enters the catalytic distillation tower 4. The steam at the bottom of the catalytic distillation tower 4 is heated, and reflux is established. The catalytic distillation tower reflux tank 5 is kept dehydrated and then enters the extraction tower 6 and the carbon four tank 7 after the reaction, and then returns to the carbon four raw material tank 1 through a pump for recycling;

[0088] The initial control flow rate is set to 0.8 cm 3 h -1 .

[0089] Specifically, see Figure 3 As shown, it is a flow chart for determining whether to start the immersion replacement mode, wherein the process of determining whether to start the immersion replacement mode according to the pretreatment monitoring result includes:

[0090] Step S210, conveying and heating the initial soaking raw material to obtain the target soaking raw material;

[0091] Step S220, real-time monitoring of the conveying process to obtain an actual monitoring image;

[0092] Step S230, real-time monitoring of the heating process to obtain the actual temperature;

[0093] Step S240, determining whether to start the immersion replacement mode according to the actual monitoring image and the actual temperature;

[0094] Wherein, the pretreatment process includes: the conveying process and the heating process.

[0095] Specifically, the process of determining whether to start the immersion replacement mode according to the actual monitoring image and the actual temperature in this embodiment includes:

[0096] Step S241, based on the actual temperature reaching a preset standard temperature variation range, determining that the actual temperature meets the kinetic energy determination condition;

[0097] Step S242, obtaining the actual maintenance time of the actual temperature meeting the kinetic energy determination condition, and determining whether the actual temperature meets the single determination condition according to the actual maintenance time;

[0098] Step S243, analyzing the actual monitoring image to obtain an actual image monitoring result, and based on the actual image monitoring result indicating that there is no foam or turbulence, determining that the actual monitoring image meets the single determination condition;

[0099] Step S244, determining whether to start the immersion replacement mode according to the actual temperature and the number of items in the actual monitoring image that meet the single determination condition, and starting the immersion replacement mode based on the number of items being 2;

[0100] Among them, based on the actual maintenance time reaching the preset standard maintenance time, it is determined that the actual temperature meets the single judgment condition; based on the actual maintenance time not reaching the standard maintenance time, it is determined that the actual temperature does not meet the single judgment condition.

[0101] Specifically, in this embodiment, based on the number of items not being 2, the immersion replacement mode is not enabled;

[0102] Based on the actual image monitoring result indicating the presence of foam or turbulence, it is determined that the actual monitoring image does not meet the single determination condition, and a first adjustment signal is issued;

[0103] adjusting the initial control flow according to the first adjustment signal to obtain the target control flow;

[0104] When the initial control flow is adjusted according to the first adjustment signal, the initial control flow is reduced according to the preset first adjustment parameter to obtain the target control flow; and adaptive selection and adjustment are performed according to the actual preparation accuracy;

[0105] In this embodiment, the first adjustment parameter is set to 0.6-0.8;

[0106] In the specific implementation process, if the initial control flow rate is 0.8cm 3 h -1 When the actual image monitoring result shows that there is foam or turbulence, the initial control flow is adjusted according to the first adjustment parameter,

[0107] 0.8cm 3 h -1 × (1-0.6) = 0.32 cm 3 h -1 ;

[0108] Among them, the first adjustment parameter is selected as 0.6;

[0109] Based on the actual monitoring image meeting the single determination condition, a first determination signal is issued;

[0110] According to the first determination signal, determining that the initial control flow is the target control flow;

[0111] Based on the fact that the actual temperature does not meet the single determination condition, the control temperature of the heating process is adjusted.

[0112] In this embodiment, the standard temperature change range is set to 30°C-60°C; the standard maintenance time is set to 2min-5min, and is adaptively selected and adjusted according to the actual preparation accuracy;

[0113] In the specific implementation process, if the actual temperature is 35°C, it is determined to be within the standard temperature change range, and the kinetic energy judgment condition is met; if the actual temperature is 10°C, the actual maintenance time is 0, that is, the actual temperature does not meet the single judgment condition, then the control temperature of the heating process is adjusted to increase the control temperature so that the actual temperature reaches the standard temperature change range as soon as possible; if the actual temperature is 80°C, the actual maintenance time is 0, that is, the actual temperature does not meet the single judgment condition, then the control temperature of the heating process is adjusted to reduce the control temperature so that the actual temperature is reduced to the standard temperature change range to avoid excessively high temperature leading to reduced activity or complete deactivation of the catalyst or causing thermal decomposition of post-ether carbon four at high temperature, producing undesirable products or by-products, affecting the quality and yield of the final product.

[0114] Specifically, the embodiments of the present invention can more accurately control the opening of the immersion replacement mode through real-time monitoring and judgment based on actual monitoring images and temperature, thereby improving the stability and repeatability of the entire process flow; detecting the presence of foam or turbulence through monitoring images and adjusting the flow rate accordingly helps to reduce or eliminate these undesirable phenomena, thereby avoiding negative impacts on product quality and process efficiency; by monitoring the actual temperature and comparing it with its standard variation range, it can ensure that the raw materials are processed at the optimal temperature, thereby optimizing reaction efficiency and product quality; by accurately controlling temperature and flow, potential safety risks caused by overheating or improper flow are reduced, thereby improving operational safety; by ensuring that the temperature is maintained at Within the actual required range, unnecessary energy consumption is avoided and operating costs are reduced; by precisely controlling the conditions of the immersion and displacement process, the quality and consistency of the final product can be improved; adaptive selection and adjustment are made according to the actual preparation accuracy, so that it can be automatically optimized according to different operating conditions, thereby improving the flexibility and adaptability of preparation; by precise control in the early stages of the process, the generation of unqualified products is reduced, thereby saving resources and reducing waste disposal costs; through automated monitoring and adjustment processes, manual intervention is reduced and production efficiency is improved; by issuing adjustment signals and confirmation signals, it is possible to respond to abnormal situations in a timely manner and take corresponding adjustment measures, thereby maintaining the continuity and stability of the production process.

[0115] See also Figure 4 As shown, it is a flow chart for determining whether the actual reaction process is qualified, wherein the process of determining whether the actual reaction process is qualified according to the actual monitoring result includes:

[0116] Step S310, real-time monitoring of the immersion and displacement process to obtain an actual pressure change rate and an actual temperature change rate;

[0117] Step S320, determining whether the actual reaction process meets the first stability condition according to the actual pressure change rate;

[0118] Step S330, determining whether the actual reaction process meets the second stability condition according to the actual temperature change rate;

[0119] Step S340: Based on the fact that the actual reaction process meets both the first stability condition and the second stability condition, it is determined that the actual reaction process is qualified.

[0120] Specifically, in this embodiment, based on the fact that the actual pressure change rate is less than or equal to the preset standard pressure change rate, it is determined that the actual pressure change rate meets the timing determination condition;

[0121] Obtaining a first maintenance time length during which the actual pressure change rate meets the timing determination condition;

[0122] Determining whether the actual reaction process meets the first stability condition according to the first maintenance time;

[0123] Comparing the first maintenance time with the standard maintenance time, and determining whether the actual reaction process meets the first stability condition according to the comparison result;

[0124] In the specific implementation process, if the first maintenance time length obtained is 30s, it does not reach the standard maintenance time length, and it is determined that the actual reaction process does not meet the first stable condition; if the first maintenance time length obtained is 7min, it reaches the standard maintenance time length, and it is determined that the actual reaction process meets the first stable condition;

[0125] Based on the fact that the actual temperature change rate is less than or equal to a preset standard temperature change rate, determining that the actual temperature change rate meets the timing determination condition;

[0126] Obtaining a second maintenance time length during which the actual temperature change rate meets the timing determination condition;

[0127] Comparing the second maintenance time with the standard maintenance time, and determining whether the actual reaction process meets the second stability condition according to the comparison result;

[0128] In the specific implementation process, if the second maintenance time length obtained is 30s, it does not reach the standard maintenance time length, and it is determined that the actual reaction process does not meet the second stable condition; if the second maintenance time length obtained is 7min, it reaches the standard maintenance time length, and it is determined that the actual reaction process meets the second stable condition;

[0129] Whether the actual reaction process meets the second stability condition is determined according to the second maintenance time.

[0130] In this embodiment, the standard pressure change rate is set to 0Pa / s-1.6Pa / s; the standard temperature change rate is set to 0°C / s-2°C / s; and adaptive selection and adjustment are performed according to actual preparation accuracy.

[0131] Specifically, the embodiments of the present invention can ensure that the reaction process is carried out under predetermined stable conditions by real-time monitoring of the pressure and temperature change rates and setting standard values, thereby improving the quality and consistency of the product; by comparing the actual maintenance time with the standard maintenance time, the reaction conditions can be adjusted in time to optimize the reaction process and reduce unnecessary fluctuations; determining whether the actual reaction process meets the stable conditions helps to promptly discover and correct potential problems, reduce risks in the production process, and avoid the production of unqualified products; by ensuring that the reaction process is carried out under stable conditions, production interruptions and product scrapping due to unstable conditions are reduced, thereby improving production efficiency.

[0132] Specifically, the process of judging whether to start the abnormality inspection mode according to the change in the water level rising speed in this embodiment includes:

[0133] Determining whether to start the abnormality inspection mode according to the change in the water level rising speed and a preset standard rising speed change;

[0134] Based on the fact that the change in the water level rising speed is less than or equal to the standard change in the water level rising speed, it is determined that the abnormality inspection mode is turned on;

[0135] Based on the fact that the change in the water level rising speed is greater than the standard change in the water level rising speed, it is determined that the verification mode is turned on;

[0136] According to the verification mode, the changes of the adjacent water level rise speeds are obtained, and the difference of the changes is calculated according to the changes of the adjacent water level rise speeds;

[0137] Determining whether to adjust the initial duration according to the change amount difference;

[0138] Based on the fact that the variation difference is less than or equal to a preset standard deviation, it is determined that the initial duration is not to be adjusted;

[0139] Based on the fact that the variation difference is greater than the standard deviation, it is determined that a second adjustment signal is sent, and the initial duration is adjusted according to the second adjustment signal to obtain an actual duration.

[0140] In the specific implementation process, based on the fact that the change in the water level rising speed is less than or equal to the standard rising speed change, it indicates that the dehydration effect is significantly reduced. Therefore, the abnormality inspection mode is turned on to determine whether an abnormality occurs in the production process or the actual dehydration process has been completed;

[0141] Since the change in the water level rising speed is greater than the standard change in the water level rising speed, it indicates that the dehydration process has not been completed and the dehydration progress has not reached the standard progress. Therefore, the verification mode is turned on, and the initial duration is reduced based on the verification mode to obtain the actual duration; by reducing the initial duration, the acquisition frequency of the periodic acquisition of the water level rising speed change is increased, thereby achieving more precise process control; facilitating timely adjustment of the production process, thereby maintaining the stability of the production process;

[0142] In this embodiment, the standard rising speed variation is set to 3 cm / h-5 cm / h; the standard deviation is set to 0.6-1, and is adaptively selected and adjusted according to the actual preparation accuracy.

[0143] Specifically, the embodiments of the present invention can timely identify potential abnormal situations and start the abnormality inspection mode by monitoring the change in the water level rise rate, thereby preventing more serious problems from occurring; by timely starting the abnormality inspection mode, measures can be quickly taken to control or stop operations that may cause danger, thereby improving the safety of the production process; by introducing the verification mode, further verification can be performed when the change in the water level rise rate exceeds the standard, so as to avoid misoperation caused by a single data point; by calculating the difference between adjacent changes in the water level rise rate, it can be more accurately determined whether the initial duration needs to be adjusted, thereby achieving more refined process control; by adjusting the initial duration to adapt to the actual water level changes, it helps to maintain the stability of the production process and reduce fluctuations.

[0144] Specifically, in this embodiment, the intermediate mixture is transported to the catalytic distillation tower 4 for catalytic distillation, and the light component is collected and reflux is established based on the catalytic distillation tower reflux tank 5 to separate the gaseous mixture, and the catalytic distillation tower reflux tank 5 is monitored in real time to obtain the actual reflux water level rising speed;

[0145] The process of collecting the actual soaking raw material after passing through the extraction tower 6 to perform the raw material circulation mode includes: recycling the actual soaking raw material to obtain the soaking raw material to be recycled, and transporting the soaking raw material to be recycled and reused as the initial soaking raw material to the pre-reactor 2;

[0146] Wherein, the actual soaking raw material is the target soaking raw material after the reaction.

[0147] Specifically, the embodiment of the present invention can more effectively separate light components in a gas mixture through the reflux operation of the reflux tank of the catalytic distillation tower, and can better control the dehydration process by real-time monitoring the reflux water level rising rate of the reflux tank of the catalytic distillation tower; determine whether to start the extraction mode based on the reflux water level rising rate, so as to ensure that the mode is started only when needed, thereby saving resources and improving efficiency; by recycling the actual soaking raw materials and recycling them as the initial soaking raw materials, it is possible to reduce the waste of raw materials and reduce production costs; the raw material circulation mode allows the production process to be carried out continuously, reduces downtime, and improves the catalyst soaking production efficiency through circulation adjustment.

[0148] The calculation compensation parameters and the calculation adjustment parameters described in the present invention have two functions: one is to balance the left and right dimensions of the formula, and the other is to adjust the numerical results. No specific assignment is performed in this embodiment. In addition, the calculation formulas in this embodiment are used to intuitively reflect the adjustment relationship between the numerical values, such as positive correlation and negative correlation. Unless otherwise specified, the parameter values ​​that are not specifically limited to numerical values ​​are all positive.

[0149] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

[0150] The above description is only a preferred embodiment of the present invention and is 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 rapid soaking method for catalysts used in MTBE production, comprising: delivering the initial soaking raw material to the pre-reactor at a preset initial controlled flow rate, and pre-treating the initial soaking raw material in the pre-reactor to obtain the target soaking raw material; Performing real-time monitoring on the pretreatment process to obtain pretreatment monitoring results, and determining whether to start the immersion replacement mode according to the pretreatment monitoring results; Based on starting the soaking and replacement mode, the target soaking raw material is delivered to the reactor at a target controlled flow rate, the initial production catalyst is soaked and replaced in the reactor according to the target soaking raw material to obtain an intermediate mixture, the soaking and replacement process is monitored in real time to obtain actual monitoring results, and whether the actual reaction process is qualified is determined according to the actual monitoring results; Based on the actual reaction process being qualified, the intermediate mixture is subjected to catalytic distillation to form a gaseous mixture; Dehydrating and extracting the gaseous mixture in sequence to obtain the actual soaking raw material; collecting the actual soaking raw materials to perform a raw material circulation mode; In the process of dehydrating the gaseous mixture, the actual reflux water level rising speed is periodically obtained with a preset initial time length, and the water level rising speed change between the actual reflux water level rising speeds at any two adjacent acquisition moments is calculated. According to the water level rising speed change, it is determined whether to start the abnormality inspection mode, and an abnormality inspection is performed on each preparation link according to the abnormality inspection mode. If each preparation link is qualified, it is determined to start the extraction mode; Each preparation link includes: a feed introduction link corresponding to the reactor for conveying the target soaking raw material, a soaking link corresponding to the reactor, and a dehydration link corresponding to the reflux tank of the catalytic distillation tower; The process of determining whether the actual reaction process is qualified according to the actual monitoring result includes: The immersion displacement process is monitored in real time to obtain the actual pressure change rate and the actual temperature change rate; Determining whether the actual reaction process meets the first stability condition according to the actual pressure change rate; Determining whether the actual reaction process meets the second stability condition according to the actual temperature change rate; Based on the fact that the actual reaction process meets both the first stability condition and the second stability condition, determining that the actual reaction process is qualified; Based on the fact that the actual pressure change rate is less than or equal to a preset standard pressure change rate, it is determined that the actual pressure change rate meets the timing determination condition; Obtaining a first maintenance time length during which the actual pressure change rate meets the timing determination condition; Determining whether the actual reaction process meets the first stability condition according to the first maintenance time; Based on the fact that the actual temperature change rate is less than or equal to a preset standard temperature change rate, determining that the actual temperature change rate meets the timing determination condition; Obtaining a second maintenance time length during which the actual temperature change rate meets the timing determination condition; determining whether the actual reaction process meets the second stability condition according to the second maintenance time; The process of judging whether to start the abnormality inspection mode according to the change in the water level rising speed includes: Determining whether to start the abnormality inspection mode according to the change in the water level rising speed and a preset standard rising speed change; Based on the fact that the change in the water level rising speed is less than or equal to the standard change in the water level rising speed, it is determined that the abnormality inspection mode is turned on; Based on the fact that the change in the water level rising speed is greater than the standard change in the water level rising speed, it is determined that the verification mode is turned on; According to the verification mode, the changes of the adjacent water level rise speeds are obtained, and the difference of the changes is calculated according to the adjacent water level rise speed changes; Determining whether to adjust the initial duration according to the change amount difference; Based on the fact that the variation difference is less than or equal to a preset standard deviation, it is determined that the initial duration is not to be adjusted; Based on the fact that the variation difference is greater than the standard deviation, it is determined that a second adjustment signal is sent, and the initial duration is adjusted according to the second adjustment signal to obtain an actual duration.

2. The rapid soaking method for MTBE production catalyst according to claim 1, characterized in that: The process of determining whether to start the immersion replacement mode according to the pretreatment monitoring result includes: The initial soaking raw material is transported and heated to obtain the target soaking raw material; Monitor the conveying process in real time to obtain actual monitoring images; Monitor the heating process in real time to obtain the actual temperature; Determining whether to start the immersion replacement mode according to the actual monitoring image and the actual temperature; Wherein, the pretreatment process includes: the conveying process and the heating process.

3. The rapid soaking method for MTBE production catalyst according to claim 2, characterized in that: The process of determining whether to start the immersion replacement mode according to the actual monitoring image and the actual temperature includes: Based on the actual temperature reaching a preset standard temperature variation range, it is determined that the actual temperature meets the kinetic energy determination condition; Obtaining an actual maintenance time during which the actual temperature meets the kinetic energy determination condition, and determining whether the actual temperature meets a single determination condition according to the actual maintenance time; Analyzing the actual monitoring image to obtain an actual image monitoring result, and determining that the actual monitoring image meets the single determination condition based on the actual image monitoring result indicating that there is no foam or turbulence; Determining whether to start the immersion replacement mode according to the actual temperature and the number of items in the actual monitoring image that meet the single determination condition, and starting the immersion replacement mode based on the number of items being 2; Among them, based on the actual maintenance time reaching the preset standard maintenance time, it is determined that the actual temperature meets the single judgment condition; based on the actual maintenance time not reaching the standard maintenance time, it is determined that the actual temperature does not meet the single judgment condition.

4. The rapid soaking method for MTBE production catalyst according to claim 3, characterized in that: Based on the actual image monitoring result indicating the presence of foam or turbulence, it is determined that the actual monitoring image does not meet the single determination condition, and a first adjustment signal is issued; adjusting the initial control flow according to the first adjustment signal to obtain the target control flow; Based on the actual monitoring image meeting the single determination condition, a first determination signal is issued; According to the first determination signal, it is determined that the initial control flow is the target control flow.

5. The rapid soaking method for MTBE production catalyst according to claim 4, characterized in that: The intermediate mixture is transported to a catalytic distillation tower for catalytic distillation, and light components are collected and reflux is established based on a reflux tank of the catalytic distillation tower to dehydrate the gaseous mixture. During the dehydration process, the reflux tank of the catalytic distillation tower is monitored in real time to obtain the actual reflux water level rising rate.

6. The rapid soaking method for the catalyst used in MTBE production according to claim 5, characterized in that: The process of collecting the actual soaking raw material to perform the raw material circulation mode includes: recycling the actual soaking raw material to obtain the soaking raw material to be recycled, and transporting the soaking raw material to be recycled and reused as the initial soaking raw material to the pre-reactor; Wherein, the actual soaking raw material is the target soaking raw material after the reaction.

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