In-situ regeneration method of molecular sieve catalyst

Abstract

The invention particularly relates to an in-situ regeneration method of a molecular sieve catalyst. The in-situ regeneration method comprises the following steps: charking regeneration preparation; setting a test group: acquiring related reaction parameter information of a test reactor and related state information of a catalyst; analyzing and processing: obtaining a device influence value and a regeneration evaluation value, and analyzing to obtain a preferred group; performing charking regeneration reaction; cooling and purging; and performing safety check. In the invention, a plurality of test groups are set, key parameters are systematically combined and tested, the most suitable regeneration condition can be accurately screened out, and the accurate parameter optimization avoids the problem of poor regeneration effect or damage to the catalyst structure caused by improper parameter selection in the traditional regeneration method. The activity and the selectivity of the catalyst can be effectively recovered after the catalyst is regenerated, so that the chemical reaction efficiency and the product quality are remarkably improved, the service life of the catalyst is prolonged, and the industrial production cost is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of catalysts, and in particular to an in-situ regeneration method for a molecular sieve catalyst. Background Art

[0002] In the modern chemical industry, molecular sieve catalysts are widely used in various chemical reaction processes.

[0003] Traditional methods of regenerating molecular sieve catalysts by charcoal burning often have many problems. On the one hand, the regeneration conditions are usually based on experience or relatively rough experimental settings, lacking precise consideration and optimization of various factors in the regeneration process. On the other hand, the existing regeneration methods have relatively simple and imperfect means of monitoring and evaluating the regeneration process. During the charcoal burning regeneration reaction, there is no comprehensive and in-depth analysis of the changes in reaction parameters such as temperature, pressure and carbon dioxide concentration in the reactor, and it is impossible to accurately judge the degree of influence of abnormal fluctuations in these parameters on the catalyst regeneration effect.

[0004] In addition, during the cooling and purging stage, the purging time is often determined based on experience or a fixed time setting, which may result in incomplete purging, and residual impurities and combustion products will affect the reusability of the catalyst; or the purging time is too long, resulting in waste of inert gas and reduced production efficiency.

[0005] Therefore, a method for in-situ regeneration of a molecular sieve catalyst is needed to solve the above-mentioned problems. Summary of the invention

[0006] The purpose of the present invention is to propose an in-situ regeneration method for a molecular sieve catalyst in order to solve the above-mentioned problem.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions: A method for in-vehicle regeneration of a molecular sieve catalyst comprises the following parts: Preparation for charcoal burning regeneration: stop feeding the reaction materials into the test reactor and the regeneration reactor, and then introduce inert gas into the test reactor and the regeneration reactor; Establishing a test group: after the inert gas replacement in the test reactor is completed, select any value from the preset temperature range, the preset oxygen concentration range, and the preset gas flow rate range to form n test groups; adjust the temperature, oxygen concentration, and gas flow rate in the test reactor to the values ​​corresponding to each test group; start burning when the carbon deposits on the catalyst reach the ignition point until the carbon burning regeneration reaction is completed, obtain the relevant reaction parameter information of the test reactor during the carbon burning reaction regeneration process in the reactor, and detect the catalyst after the carbon burning regeneration reaction to obtain the catalyst related status information; Analysis and processing: Analyze the relevant state information of the charcoal burning regeneration process in the test reactor in each test group and the relevant state information of the catalyst to obtain the reactor impact value and the regeneration evaluation value respectively; after comprehensively analyzing the obtained regeneration evaluation value and reactor impact value, select the corresponding test group as the preferred group; Carbon burning regeneration reaction: After the inert gas replacement in the regeneration reactor is completed, a gas with a preferred oxygen concentration is introduced into the reactor at a preferred gas flow rate, and the regeneration reactor is heated to a preferred temperature at the same time, and the pressure of the regeneration reactor is kept stable until the carbon burning regeneration reaction in the regeneration reactor is completed; Cooling and purging: After the carbon deposits are burned, stop introducing the gas with the preferred oxygen concentration into the regeneration reactor, introduce inert gas into the regeneration reactor and cool the regeneration reactor, so that the temperature of the regeneration reactor gradually decreases to room temperature, and then continue to purge the catalyst bed in the regeneration reactor with inert gas for a preferred time until the impurities and combustion products remaining in the carbon burning regeneration process are completely removed; Safety check: Check the regeneration reactor to ensure that it returns to normal.

[0008] Preferably, the reaction parameter information related to the test reactor during the charcoal burning reaction regeneration process includes: The carbon dioxide concentration at the outlet of the test reactor, the regeneration time zone, and the temperature and pressure of the test reactor in the regeneration time zone; wherein the regeneration time zone is timed from the moment when the charcoal burning regeneration reaction starts, until the carbon dioxide concentration is lower than the preset reference concentration and remains below the preset time, marking the end of the time; Catalyst related status information includes: After the charcoal burning regeneration reaction, the catalyst weight and the particle size of the catalyst particles in the reactor were tested.

[0009] Preferably, the catalyst-related state information is analyzed, and the specific process is as follows: Weigh the catalyst of any test group and record the weighed weight as the reference weight; place the weighed catalyst in a fixed bed reactor, introduce a set amount of alkaline gas, place it at a preset temperature, and wait for the alkaline gas to be adsorbed on the catalyst surface; The adsorbate concentration of the catalyst in the fixed bed reactor is detected at a set time period. When the concentration fluctuation within a preset time interval is less than a preset allowable fluctuation range, it is the adsorption equilibrium moment; the catalyst weight at the adsorption equilibrium moment is recorded and the difference between it and the reference weight is calculated to obtain the adsorption mass; The catalyst in the fixed bed reactor is heated to the temperature corresponding to the test group at a set heating rate, and the desorption peaks appearing when the temperature is raised to the temperature corresponding to the test group and the molecular weight of the adsorbate corresponding to each desorption peak are recorded, and the molecular weight of the adsorbate corresponding to all the desorption peaks when the temperature is raised to the temperature corresponding to the test group are summed up to calculate the total molecular weight of the adsorbate; The ratio of the molecular weight of the adsorbate corresponding to the desorption peak at the temperature corresponding to the test group to the total molecular weight of the adsorbate is recorded as the adsorbate ratio; The weight factors corresponding to the adsorption mass and the adsorbate ratio are preset, and the energy efficiency value is obtained by multiplying the adsorption mass and the adsorbate ratio with the corresponding weight factors, and then the energy efficiency value of each test group is obtained in turn.

[0010] Preferably, the analysis of the catalyst-related state information further includes the following parts: Using a laser particle size analyzer to obtain the particle size of the catalyst particles in any test group, establishing a standard particle size of the catalyst particles, comparing the particle size of the catalyst particles in the test group with the standard particle size, marking the catalyst particles larger than the standard particle size as abnormal particles, and recording the difference between the particle size of the abnormal particles and the particle size of the standard particles as the abnormal difference; The abnormal difference is matched with the preset three groups of threshold value ranges, and the three groups of threshold value ranges are set to correspond to a particle size level respectively, so as to obtain the particle size level corresponding to the abnormal difference, wherein the particle size level includes a mild abnormal level, a moderate abnormal level and a severe abnormal level; The weights of all abnormal particles in the mild abnormality level, the moderate abnormality level, and the severe abnormality level are summed up in turn to obtain the total weight of mild abnormal particles, the total weight of moderate abnormal particles, and the total weight of severe abnormal particles; Preset the weight factors corresponding to the mild abnormality level, the moderate abnormality level and the severe abnormality level, respectively, and multiply the total weight of mild abnormal particles / total weight of catalyst, the total weight of moderate abnormal particles / total weight of catalyst and the total weight of severe abnormal particles / total weight of catalyst with their corresponding weight factors and then sum them to obtain the abnormal weight value; The specific gravity value and energy efficiency value are marked as and Then perform weighted calculation using the formula: ; Get the regeneration evaluation value ;in and are the weight factors corresponding to the different weight values ​​and the energy efficiency values ​​respectively; and the regeneration evaluation values ​​of each test group are obtained in turn.

[0011] Preferably, the relevant state information of the charcoal burning regeneration process in the test reactor in each test group is analyzed, and the specific process is as follows: The corresponding temperature value in the test group is recorded as the reference temperature value, and the temperature value of the test reactor in the regeneration time zone that is greater than the reference temperature is marked as an abnormally high temperature value; the number of all abnormally high temperature values ​​in the regeneration time zone is counted and recorded as the abnormally high temperature value; Obtaining the abnormally high temperature frequency of the test reactor in the regeneration time zone based on the abnormally high temperature value and the regeneration time zone; The time from when the temperature of the test reactor starts to rise from the reference temperature value to when it is greater than the reference temperature value and then drops to the reference temperature value is recorded as the duration; all durations in the regeneration time zone are accumulated to obtain the abnormal duration corresponding to the abnormally high temperature value; The abnormal high temperature value, abnormal high temperature frequency, and abnormal duration are marked as , , Then perform weighted calculation using the formula: ; Get the temperature difference ;in , and They are the temperature value corresponding to the test group, the maximum frequency allowed for abnormally high temperatures, and the maximum duration of abnormality; , , They are the weight factors corresponding to the abnormal high temperature value, abnormal high temperature frequency, and abnormal duration; According to the above process of analyzing the temperature in the test reactor during the charcoal burning regeneration process to obtain the temperature difference value, the pressure in the test reactor during the charcoal burning regeneration process is analyzed to obtain the pressure difference value; The weight factors corresponding to the preset temperature difference value and the pressure difference value are respectively calculated, and the temperature difference value and the pressure difference value are respectively multiplied by the corresponding weight factors and then summed to obtain the device influence value.

[0012] Preferably, the regeneration evaluation values ​​of each test group are arranged in descending order according to size to obtain a regeneration evaluation value descending set, and the device impact value corresponding to each regeneration evaluation value in the regeneration evaluation value descending set is obtained; Set up the device impact threshold, and compare the device impact value corresponding to the regeneration evaluation value with its threshold in descending order from left to right: If the device impact value is less than or equal to its threshold value, the test group corresponding to the device impact value is marked as the preferred group, and the temperature, oxygen concentration and gas flow rate corresponding to the parameter combination of the preferred group are respectively used as the preferred temperature, oxygen concentration and gas flow rate for charcoal regeneration in the catalyst device; If the device impact value is greater than its threshold, the regeneration evaluation value corresponding to the device impact value and its corresponding test group parameter combination will be eliminated, and the device impact value of the next regeneration evaluation value will be compared and judged with its threshold in the order of the regeneration evaluation values. The above judgment process will be repeated until the preferred group that meets the conditions is screened out.

[0013] Preferably, the specific process of obtaining the preferred time is as follows: After the charcoal burning regeneration reaction in any regeneration reactor is completed and the temperature of the regeneration reactor is gradually reduced to room temperature, the catalyst is taken out and evenly divided into several groups according to the quality; each group of catalysts is placed in the corresponding detection reactor in turn; Purging the catalyst bed in each detection reactor, recording the start time of the purging as the start time, and monitoring the concentration of carbon deposit particles, carbon monoxide and carbon dioxide at the outlet of the detection reactor; The standard values ​​of carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at the outlet of the detection reactor are respectively set, and the time point when the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at the outlet of the detection reactor are all lower than the corresponding standard values ​​is marked as T1; The time point after T1 when the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration are all lower than the corresponding standard value for the set number of times is marked as T2, and the time period between T1 and T2 is recorded as the waiting time period; Obtaining the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration corresponding to each time point in the waiting time zone, and performing difference calculations on the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at each time point and their corresponding standard values ​​respectively to obtain the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference respectively; The weight factors corresponding to the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference are preset respectively, and the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference are multiplied by their corresponding weight factors and then summed to obtain the qualified value, and the qualified value at each time point is obtained in turn; the maximum allowable value corresponding to the preset qualified value is marked, and the result of the maximum allowable value / qualified value is marked as the qualified ratio.

[0014] Preferably, the process of obtaining the preferred time also includes the following parts: According to the process of analyzing the catalyst-related state information to obtain the regeneration evaluation value, the catalyst taken out at each time point in the timing zone is analyzed to obtain the regeneration evaluation value of the catalyst at each time point, and it is marked as the catalytic state value; Obtain the inert gas consumption for purging corresponding to each time point and preset the standard consumption of the inert gas, and mark the ratio result of the inert gas consumption for purging / the preset standard consumption of the inert gas as the consumption ratio; The catalytic state value, qualified ratio value, and consumption ratio value are marked as , and Then perform weighted calculation using the formula: ; Get the purge value ,in , and are the weight factors corresponding to the catalytic state value, qualified ratio, and consumption ratio respectively; the time between the time point corresponding to the maximum purge comprehensive value and the start time is marked as the preferred time.

[0015] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are: 1. The present invention sets up multiple test groups and systematically combines and tests key parameters, so as to accurately screen out the most suitable regeneration conditions. This precise parameter optimization avoids the problems of poor regeneration effect or damage to the catalyst structure caused by improper parameter selection in traditional regeneration methods, so that the catalyst can more effectively restore its activity and selectivity after regeneration, thereby significantly improving the efficiency of chemical reactions and product quality, extending the service life of the catalyst, and reducing industrial production costs.

[0016] 2. The present invention determines the optimal time for the cooling and purging stage by analyzing the state of the catalyst, which can ensure that the impurities and combustion products remaining in the charcoal burning regeneration process are completely removed and the reusability of the catalyst is not affected, and avoids the waste of inert gas and reduced production efficiency caused by excessive purging, thereby rationally utilizing resources and providing strong support for the sustainable development of industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Further details, features and advantages of the present application are disclosed in the following description of exemplary embodiments in conjunction with the accompanying drawings, in which: Figure 1 The figure is a flow chart of the method of the present invention. DETAILED DESCRIPTION

[0018] Several embodiments of the present application will be described in more detail below with reference to the accompanying drawings so that those skilled in the art can implement the present application. The present application can be embodied in many different forms and purposes and should not be limited to the embodiments described herein. These embodiments are provided to make the present application comprehensive and complete, and to fully convey the scope of the present application to those skilled in the art. The embodiments do not limit the present application.

[0019] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by those of ordinary skill in the art to which this application belongs. It will be further understood that terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with their meaning in the relevant art and / or the context of this specification, and will not be interpreted in an idealized or overly formal sense unless explicitly defined as such herein.

[0020] See also Figure 1 As shown, the present invention provides a technical solution: A method for in-vehicle regeneration of a molecular sieve catalyst comprises the following parts: Preparation for charcoal burning regeneration: stop feeding the reaction materials into the test reactor and the regeneration reactor, and then introduce inert gas into the test reactor and the regeneration reactor; Establishing a test group: after the inert gas replacement in the test reactor is completed, select any value from the preset temperature range, preset oxygen concentration range, and preset gas flow rate range to form n test groups, where n is the total number of test groups and is set by the technician; adjust the temperature, oxygen concentration, and gas flow rate in the test reactor to the values ​​corresponding to each test group; start burning when the carbon deposits on the catalyst reach the ignition point until the carbonization regeneration reaction is completed, obtain the relevant reaction parameter information of the test reactor during the carbonization reaction regeneration process in the reactor, and detect the catalyst after the carbonization regeneration reaction to obtain the catalyst-related status information; The relevant reaction parameter information of the test reactor during the charcoal burning reaction regeneration process includes: The carbon dioxide concentration at the outlet of the test reactor, the regeneration time zone, and the temperature and pressure of the test reactor in the regeneration time zone; wherein the regeneration time zone is timed from the moment when the charcoal burning regeneration reaction starts, until the carbon dioxide concentration is lower than the preset reference concentration and remains below the preset time, marking the end of the time; The catalyst-related status information includes: the catalyst weight and the particle size of the catalyst particles in the test reactor after the charcoal burning regeneration reaction; The catalyst-related status information is analyzed, and the specific process is as follows: Weigh the catalyst of any test group and record the weighed weight as the reference weight; place the weighed catalyst in a fixed bed reactor, introduce a set amount of alkaline gas, place it at a preset temperature, and wait for the alkaline gas to be adsorbed on the catalyst surface; The adsorbate concentration of the catalyst in the fixed bed reactor is detected at a set time period. When the concentration fluctuation within a preset time interval is less than a preset allowable fluctuation range, it is the adsorption equilibrium moment; the catalyst weight at the adsorption equilibrium moment is recorded and the difference between it and the reference weight is calculated to obtain the adsorption mass; The catalyst in the fixed bed reactor is heated to the temperature corresponding to the test group at a set heating rate, and the desorption peaks appearing when the temperature is raised to the temperature corresponding to the test group and the molecular weight of the adsorbate corresponding to each desorption peak are recorded, and the molecular weight of the adsorbate corresponding to all the desorption peaks when the temperature is raised to the temperature corresponding to the test group are summed up to calculate the total molecular weight of the adsorbate; The ratio of the molecular weight of the adsorbate corresponding to the desorption peak at the temperature corresponding to the test group to the total molecular weight of the adsorbate is recorded as the adsorbate ratio; Preset the weight factors corresponding to the adsorption mass and the adsorbate ratio, respectively, multiply the adsorption mass and the adsorbate ratio by the corresponding weight factors, and then sum them to obtain the energy efficiency value, and obtain the energy efficiency value of each test group in turn; Using a laser particle size analyzer to obtain the particle size of the catalyst particles in any test group, establishing a standard particle size of the catalyst particles, comparing the particle size of the catalyst particles in the test group with the standard particle size, marking the catalyst particles larger than the standard particle size as abnormal particles, and recording the difference between the particle size of the abnormal particles and the particle size of the standard particles as the abnormal difference; The abnormal difference is matched with the preset three groups of threshold value ranges, and the three groups of threshold value ranges are set to correspond to a particle size level respectively, so as to obtain the particle size level corresponding to the abnormal difference, wherein the particle size level includes a mild abnormal level, a moderate abnormal level and a severe abnormal level; The weights of all abnormal particles in the mild abnormality level, the moderate abnormality level, and the severe abnormality level are summed up in turn to obtain the total weight of mild abnormal particles, the total weight of moderate abnormal particles, and the total weight of severe abnormal particles; Preset the weight factors corresponding to the mild abnormality level, the moderate abnormality level and the severe abnormality level, respectively, and multiply the total weight of mild abnormal particles / total weight of catalyst, the total weight of moderate abnormal particles / total weight of catalyst and the total weight of severe abnormal particles / total weight of catalyst with their corresponding weight factors and then sum them to obtain the abnormal weight value; The specific gravity value and energy efficiency value are marked as and Then perform weighted calculation using the formula: ; Get the regeneration evaluation value ;in and are weight factors corresponding to the different weight values ​​and energy efficiency values ​​respectively; and the regeneration evaluation values ​​of each test group are obtained in turn; Analysis and processing: Analyze the relevant state information of the charcoal burning regeneration process in the test reactor in each test group and the relevant state information of the catalyst to obtain the reactor impact value and the regeneration evaluation value respectively; after comprehensively analyzing the obtained regeneration evaluation value and reactor impact value, select the corresponding test group as the preferred group; The relevant status information of the charcoal burning regeneration process in the test reactor in each test group is analyzed. The specific process is as follows: The corresponding temperature value in the test group is recorded as the reference temperature value, and the temperature value of the test reactor in the regeneration time zone that is greater than the reference temperature is marked as an abnormally high temperature value; the number of all abnormally high temperature values ​​in the regeneration time zone is counted and recorded as the abnormally high temperature value; Obtaining the abnormally high temperature frequency of the test reactor in the regeneration time zone based on the abnormally high temperature value and the regeneration time zone; The time from when the temperature of the test reactor starts to rise from the reference temperature value to when it is greater than the reference temperature value and then drops to the reference temperature value is recorded as the duration; all durations in the regeneration time zone are accumulated to obtain the abnormal duration corresponding to the abnormally high temperature value; The abnormal high temperature value, abnormal high temperature frequency, and abnormal duration are marked as , , Then perform weighted calculation using the formula: ; Get the temperature difference ;in , and They are the temperature value corresponding to the test group, the maximum frequency allowed for abnormally high temperatures, and the maximum duration of abnormality; , , They are the weight factors corresponding to the abnormal high temperature value, abnormal high temperature frequency, and abnormal duration; According to the above process of analyzing the temperature in the test reactor during the charcoal burning regeneration process to obtain the temperature difference value, the pressure in the test reactor during the charcoal burning regeneration process is analyzed to obtain the pressure difference value; Preset the weight factors corresponding to the temperature difference value and the pressure difference value, respectively, and calculate the product of the temperature difference value and the pressure difference value and their corresponding weight factors and then sum them to obtain the device influence value; Arrange the regeneration evaluation values ​​of each test group in descending order according to size to obtain a regeneration evaluation value descending set, and obtain the device impact value corresponding to each regeneration evaluation value in the regeneration evaluation value descending set; Set up the device impact threshold, and compare the device impact value corresponding to the regeneration evaluation value with its threshold in descending order from left to right: If the device influence value is less than or equal to its threshold value, it indicates that under the test group parameter combination corresponding to the device influence value, the reactor can stably maintain operation under the parameter conditions set by the test group during the charcoal burning regeneration process. Therefore, the test group corresponding to the device influence value is marked as the preferred group, and the temperature, oxygen concentration and gas flow rate corresponding to the preferred group parameter combination are respectively used as the preferred temperature, oxygen concentration and gas flow rate for charcoal burning regeneration in the catalyst device; If the device influence value is greater than its threshold value, it indicates that under the parameter combination of the test group corresponding to the device influence value, the reactor cannot stably maintain operation under the parameter conditions set by the test group during the charcoal burning regeneration process. Therefore, the regeneration evaluation value corresponding to the device influence value and its corresponding test group parameter combination are eliminated, and the device influence value of the next regeneration evaluation value is compared and judged with its threshold value in the order of the regeneration evaluation value sequence, and the above judgment process is repeated until the preferred group that meets the conditions is screened out; Carbon burning regeneration reaction: After the inert gas replacement in the regeneration reactor is completed, a gas with a preferred oxygen concentration is introduced into the reactor at a preferred gas flow rate, and the regeneration reactor is heated to a preferred temperature at the same time, and the pressure of the regeneration reactor is kept stable until the carbon burning regeneration reaction in the regeneration reactor is completed; Cooling and purging: After the carbon deposits are burned, stop introducing the gas with the preferred oxygen concentration into the regeneration reactor, introduce inert gas into the regeneration reactor and cool the regeneration reactor, so that the temperature of the regeneration reactor gradually decreases to room temperature, and then continue to purge the catalyst bed in the regeneration reactor with inert gas for a preferred time until the impurities and combustion products remaining in the carbon burning regeneration process are completely removed; The specific process of obtaining the preferred time is as follows: After the charcoal burning regeneration reaction in any regeneration reactor is completed and the temperature of the regeneration reactor is gradually reduced to room temperature, the catalyst is taken out and evenly divided into several groups according to the quality; each group of catalysts is placed in the corresponding detection reactor in turn; Purging the catalyst bed in each detection reactor, recording the start time of the purging as the start time, and monitoring the concentration of carbon deposit particles, carbon monoxide and carbon dioxide at the outlet of the detection reactor; The standard values ​​of carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at the outlet of the detection reactor are respectively set, and the time point when the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at the outlet of the detection reactor are all lower than the corresponding standard values ​​is marked as T1; The time point after T1 when the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration are all lower than the corresponding standard value for the set number of times is marked as T2, and the time period between T1 and T2 is recorded as the waiting time period; Obtaining the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration corresponding to each time point in the waiting time zone, and performing difference calculations on the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at each time point and their corresponding standard values ​​respectively to obtain the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference respectively; The weight factors corresponding to the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference are preset respectively, and the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference are multiplied by their corresponding weight factors and then summed to obtain the qualified value, and the qualified value at each time point is obtained in turn; the maximum allowable value corresponding to the preset qualified value is marked, and the result of the maximum allowable value / qualified value is marked as the qualified ratio.

[0021] The process of obtaining the preferred time also includes the following parts: According to the process of analyzing the catalyst-related state information to obtain the regeneration evaluation value, the catalyst taken out at each time point in the timing zone is analyzed to obtain the regeneration evaluation value of the catalyst at each time point, and it is marked as the catalytic state value; Obtain the inert gas consumption for purging corresponding to each time point and preset the standard consumption of the inert gas, and mark the ratio result of the inert gas consumption for purging / the preset standard consumption of the inert gas as the consumption ratio; The catalytic state value, qualified ratio value, and consumption ratio value are marked as , and Then perform weighted calculation using the formula: ; Get the purge value ,in , and are weight factors corresponding to the catalytic state value, qualified ratio, and consumption ratio respectively; the time between the time point corresponding to the maximum purge comprehensive value and the start time is marked as the preferred time; Safety check: Check the regeneration reactor to ensure that it returns to normal.

[0022] The inspection of the regeneration reactor includes: checking the sealing through pressure test, checking the pressure change to determine whether there is a risk of leakage, and repairing the sealing parts as needed; then checking the internal parts, checking whether the inner wall has cracks, deformation, corrosion, the mechanical structure integrity and lubrication of the stirring device, sensor calibration and function test, auxiliary equipment connection, valve, instrument condition, electrical equipment insulation, grounding, etc., and confirming that the surrounding safety protection facilities are intact. The reactor can be put into subsequent use only after all indicators meet the safety requirements.

[0023] The above formulas are obtained by collecting a large amount of data and performing software simulation, and a formula close to the actual value is selected. The influencing weight factor and specific coefficient value in the formula are set by technical personnel in this field according to actual conditions, and can be adjusted and modified later.

[0024] The above description of the embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for in-situ regeneration of a molecular sieve catalyst, characterized in that: Includes the following sections: Preparation for charcoal burning regeneration: stop feeding the reaction materials into the test reactor and the regeneration reactor, and then introduce inert gas into the test reactor and the regeneration reactor; Establishing a test group: after the inert gas replacement in the test reactor is completed, select any value from the preset temperature range, the preset oxygen concentration range, and the preset gas flow rate range to form n test groups; adjust the temperature, oxygen concentration, and gas flow rate in the test reactor to the values ​​corresponding to each test group; start burning when the carbon deposits on the catalyst reach the ignition point until the carbon burning regeneration reaction is completed, obtain the relevant reaction parameter information of the test reactor during the carbon burning reaction regeneration process in the reactor, and detect the catalyst after the carbon burning regeneration reaction to obtain the catalyst related status information; Analysis and processing: Analyze the relevant state information of the charcoal burning regeneration process in the test reactor in each test group and the relevant state information of the catalyst to obtain the reactor impact value and the regeneration evaluation value respectively; after comprehensively analyzing the obtained regeneration evaluation value and reactor impact value, select the corresponding test group as the preferred group; Carbon burning regeneration reaction: After the inert gas replacement in the regeneration reactor is completed, a gas with a preferred oxygen concentration is introduced into the reactor at a preferred gas flow rate, and the regeneration reactor is heated to a preferred temperature at the same time, and the pressure of the regeneration reactor is kept stable until the carbon burning regeneration reaction in the regeneration reactor is completed; Cooling and purging: After the carbon deposits are burned, stop introducing the gas with the preferred oxygen concentration into the regeneration reactor, introduce inert gas into the regeneration reactor and cool the regeneration reactor, so that the temperature of the regeneration reactor gradually decreases to room temperature, and then continue to purge the catalyst bed in the regeneration reactor with inert gas for a preferred time until the impurities and combustion products remaining in the carbon burning regeneration process are completely removed; Safety check: Check the regeneration reactor to ensure that it returns to normal.

2. The in-situ regeneration method of a molecular sieve catalyst according to claim 1, characterized in that: The relevant reaction parameter information of the test reactor during the charcoal burning reaction regeneration process includes: The carbon dioxide concentration at the outlet of the test reactor, the regeneration time zone, and the temperature and pressure of the test reactor in the regeneration time zone; wherein the regeneration time zone is timed from the moment when the charcoal burning regeneration reaction starts, until the carbon dioxide concentration is lower than the preset reference concentration and remains below the preset time, marking the end of the time; Catalyst related status information includes: After the charcoal burning regeneration reaction, the catalyst weight and the particle size of the catalyst particles in the reactor were tested.

3. The in-situ regeneration method of a molecular sieve catalyst according to claim 2, characterized in that: The specific process of analyzing the catalyst related status information is as follows: Weigh the catalyst of any test group and record the weighed weight as the reference weight; place the weighed catalyst in a fixed bed reactor, introduce a set amount of alkaline gas, place it at a preset temperature, and wait for the alkaline gas to be adsorbed on the catalyst surface; The adsorbate concentration of the catalyst in the fixed bed reactor is detected at a set time period. When the concentration fluctuation within a preset time interval is less than a preset allowable fluctuation range, it is the adsorption equilibrium moment; the catalyst weight at the adsorption equilibrium moment is recorded and the difference between it and the reference weight is calculated to obtain the adsorption mass; The catalyst in the fixed bed reactor is heated to the temperature corresponding to the test group at a set heating rate, and the desorption peaks appearing when the temperature is raised to the temperature corresponding to the test group and the molecular weight of the adsorbate corresponding to each desorption peak are recorded, and the molecular weight of the adsorbate corresponding to all the desorption peaks when the temperature is raised to the temperature corresponding to the test group are summed up to calculate the total molecular weight of the adsorbate; The ratio of the molecular weight of the adsorbate corresponding to the desorption peak at the temperature corresponding to the test group to the total molecular weight of the adsorbate is recorded as the adsorbate ratio; The weight factors corresponding to the adsorption mass and the adsorbate ratio are preset, and the energy efficiency value is obtained by multiplying the adsorption mass and the adsorbate ratio with the corresponding weight factors, and then the energy efficiency value of each test group is obtained in turn.

4. The in-situ regeneration method of a molecular sieve catalyst according to claim 3, characterized in that: The analysis of the catalyst related status information also includes the following parts: Using a laser particle size analyzer to obtain the particle size of the catalyst particles in any test group, establishing a standard particle size of the catalyst particles, comparing the particle size of the catalyst particles in the test group with the standard particle size, marking the catalyst particles larger than the standard particle size as abnormal particles, and recording the difference between the particle size of the abnormal particles and the particle size of the standard particles as the abnormal difference; The abnormal difference is matched with the preset three groups of threshold value ranges, and the three groups of threshold value ranges are set to correspond to a particle size level respectively, so as to obtain the particle size level corresponding to the abnormal difference, wherein the particle size level includes a mild abnormal level, a moderate abnormal level and a severe abnormal level; The weights of all abnormal particles in the mild abnormality level, the moderate abnormality level, and the severe abnormality level are summed up in turn to obtain the total weight of mild abnormal particles, the total weight of moderate abnormal particles, and the total weight of severe abnormal particles; Preset the weight factors corresponding to the mild abnormality level, the moderate abnormality level and the severe abnormality level, respectively, and multiply the total weight of mild abnormal particles / total weight of catalyst, the total weight of moderate abnormal particles / total weight of catalyst and the total weight of severe abnormal particles / total weight of catalyst with their corresponding weight factors and then sum them to obtain the abnormal weight value; The specific gravity value and energy efficiency value are marked as and Then perform weighted calculation using the formula: ； Get the regeneration evaluation value ;in and are the weight factors corresponding to the different weight values ​​and the energy efficiency values ​​respectively; and the regeneration evaluation values ​​of each test group are obtained in turn.

5. The in-situ regeneration method of a molecular sieve catalyst according to claim 4, characterized in that: The relevant state information of the charcoal burning regeneration process in the test reactor in each test group is analyzed, and the specific process is as follows: The corresponding temperature value in the test group is recorded as the reference temperature value, and the temperature value of the test reactor in the regeneration time zone that is greater than the reference temperature is marked as an abnormally high temperature value; the number of all abnormally high temperature values ​​in the regeneration time zone is counted and recorded as the abnormally high temperature value; Obtaining the abnormally high temperature frequency of the test reactor in the regeneration time zone based on the abnormally high temperature value and the regeneration time zone; The time from when the temperature of the test reactor starts to increase from the reference temperature value to when it is greater than the reference temperature value and then decreases to the reference temperature value is recorded as the duration; All durations in the regeneration time zone are accumulated to obtain the abnormal duration corresponding to the abnormal high temperature value; The abnormal high temperature value, abnormal high temperature frequency, and abnormal duration are marked as , , Then perform weighted calculation using the formula: ； Get the temperature difference ;in , and They are the temperature value corresponding to the test group, the maximum frequency allowed for abnormally high temperatures, and the maximum duration of abnormality; , , They are the weight factors corresponding to the abnormal high temperature value, abnormal high temperature frequency, and abnormal duration; According to the above process of analyzing the temperature in the test reactor during the charcoal burning regeneration process to obtain the temperature difference value, the pressure in the test reactor during the charcoal burning regeneration process is analyzed to obtain the pressure difference value; The weight factors corresponding to the preset temperature difference value and the pressure difference value are respectively calculated, and the temperature difference value and the pressure difference value are respectively multiplied by the corresponding weight factors and then summed to obtain the device influence value.

6. The in-situ regeneration method of a molecular sieve catalyst according to claim 5, characterized in that: The regeneration evaluation values ​​of each test group are arranged in descending order according to their size to obtain a regeneration evaluation value descending set, and the device impact value corresponding to each regeneration evaluation value in the regeneration evaluation value descending set is obtained; Set up the device impact threshold, and compare the device impact value corresponding to the regeneration evaluation value with its threshold in descending order from left to right: If the influence value of the catalyst is less than or equal to the threshold value, the temperature, oxygen concentration and gas flow rate corresponding to the optimal group of parameter combinations are respectively used as the optimal temperature, oxygen concentration and gas flow rate for charcoal regeneration in the catalyst; If the device impact value is greater than its threshold, the regeneration evaluation value corresponding to the device impact value and its corresponding test group parameter combination will be eliminated, and the device impact value of the next regeneration evaluation value will be compared and judged with its threshold in the order of the regeneration evaluation values. The above judgment process will be repeated until the preferred group that meets the conditions is screened out.

7. The in-situ regeneration method of a molecular sieve catalyst according to claim 6, characterized in that: The specific process of obtaining the preferred time is as follows: After the charcoal burning regeneration reaction in any regeneration reactor is completed and the temperature of the regeneration reactor is gradually reduced to room temperature, the catalyst is taken out and evenly divided into several groups according to the quality; each group of catalysts is placed in the corresponding detection reactor in turn; Purging the catalyst bed in each detection reactor, recording the start time of the purging as the start time, and monitoring the concentration of carbon deposit particles, carbon monoxide and carbon dioxide at the outlet of the detection reactor; The standard values ​​of carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at the outlet of the detection reactor are respectively set, and the time point when the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at the outlet of the detection reactor are all lower than the corresponding standard values ​​is marked as T1; The time point after T1 when the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration are all lower than the corresponding standard value for the set number of times is marked as T2, and the time period between T1 and T2 is recorded as the waiting time period; Obtaining the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration corresponding to each time point in the waiting time zone, and performing difference calculations on the carbon deposit particle concentration, carbon monoxide concentration and carbon dioxide concentration at each time point and their corresponding standard values ​​respectively to obtain the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference respectively; Preset weight factors corresponding to carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference respectively, multiply the carbon deposit particle concentration difference, carbon monoxide concentration difference and carbon dioxide concentration difference by their corresponding weight factors respectively, and then sum them to obtain qualified values, and obtain qualified values ​​at each time point in turn; The maximum allowable value corresponding to the preset qualified value is marked as the qualified ratio by dividing the maximum allowable value by the qualified value.

8. The in-situ regeneration method of a molecular sieve catalyst according to claim 7, characterized in that: The process of obtaining the preferred time also includes the following parts: According to the process of analyzing the catalyst-related state information to obtain the regeneration evaluation value, the catalyst taken out at each time point in the timing zone is analyzed to obtain the regeneration evaluation value of the catalyst at each time point, and it is marked as the catalytic state value; Obtain the inert gas consumption for purging corresponding to each time point and preset the standard consumption of the inert gas, and mark the ratio result of the inert gas consumption for purging / the preset standard consumption of the inert gas as the consumption ratio; The catalytic state value, qualified ratio value, and consumption ratio value are marked as , and Then perform weighted calculation using the formula: ； Get the total purge value ,in , and are the weight factors corresponding to the catalytic state value, qualified ratio, and consumption ratio respectively; the time between the time point corresponding to the maximum purge comprehensive value and the start time is marked as the preferred time.

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