A high-performance composite modified calcined petroleum coke and its preparation method

Abstract

The present application relates to the field of petroleum coke preparation, and specifically to a high-performance composite modified calcined petroleum coke and a preparation method thereof. The method comprises: stirring calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride, and sodium silicate, performing an intercalation reaction, obtaining temperature difference samples at each sampling moment, and combining them with anomaly detection to obtain segmented samples; dividing the sintering furnace temperature control process based on the segmented samples, determining the temperature difference matrix for each interval, and obtaining response difference values for each batch; adjusting the parameters of the sintering furnace temperature control for the current batch to obtain a graphite intercalation compound; and after ball milling the graphite intercalation compound, adding a base material, water-soluble cellulose ether, sodium silicate, and calcium oxide, and continuing to stir and mix to obtain a high-performance composite modified petroleum coke. This application aims to avoid the situation where the product intercalation degree is uneven due to uneven sintering reaction temperature.

Description

Technical Field

[0001] The present application relates to the field of petroleum coke preparation, and in particular to a high-performance composite modified calcined petroleum coke and a preparation method thereof. Background Art

[0002] With the rapid development of modern industry, the demand for high-performance carbonaceous materials continues to rise across many industries. In the aluminum smelting industry, high-quality carbonaceous anode materials play a vital role in reducing energy consumption, improving aluminum purity, and enhancing production efficiency. In battery manufacturing, high-performance carbon anode materials can significantly enhance the battery's charge and discharge performance and extend its service life. Calcined petroleum coke, as an important carbonaceous raw material, is widely used in the aforementioned industries due to its outstanding advantages, such as good conductivity and high carbon content. However, traditional calcined petroleum coke has certain performance shortcomings. For example, when its sulfur content is high, pollutant gases are released during use, which not only negatively affects product quality but also has adverse effects on the environment. At the same time, its pore structure and micromorphology cannot fully meet the stringent requirements of specific application scenarios.

[0003] To effectively address these issues, the production technology for composite-modified calcined petroleum coke has emerged. By implementing composite modification on calcined petroleum coke, its physical and chemical properties can be effectively optimized, enhancing its application value across various industries and thus meeting the ever-evolving demands of industrial production. Currently, the production process for calcined petroleum coke is automated. However, during the production of different batches of material, significant differences in equipment parameter responses across different stages of production and preparation lead to uneven sintering reaction temperatures, resulting in varying degrees of intercalation in the product, which in turn affects the uniformity of product quality and performance. Summary of the Invention

[0004] In view of the above, it is necessary to provide a high-performance composite modified calcined petroleum coke and a preparation method thereof to solve the above problems.

[0005] The first aspect of the present application provides a method for preparing high-performance composite modified calcined petroleum coke, the method comprising:

[0006] Calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride, and sodium silicate are mixed and stirred, and the stirred mixture is placed in batches into a sintering furnace for intercalation reaction. The temperature difference between the temperature data at each acquisition moment and the preset temperature data is obtained, and all the temperature differences in the same order across all batches are combined into a temperature difference sample. All the temperature difference samples are mapped and combined with anomaly detection to obtain segmented samples;

[0007] The sintering furnace temperature control process is divided based on the segmented samples, and the temperature difference samples corresponding to the divided intervals are combined to determine the temperature difference matrix of each divided interval, and the responses of different batches to the temperature control in the temperature difference matrix are compared. The response difference value of each batch is obtained based on the data change trend of the temperature difference matrix; the parameters of the sintering furnace temperature control of the current batch are adjusted according to the response difference value of the previous batch of the current batch to obtain the graphite intercalation compound;

[0008] After the graphite intercalation compound is crushed by ball milling, base material, water-soluble cellulose ether, sodium silicate and calcium oxide are added and stirred and mixed continuously. The mixed materials are mechanically granulated and packaged to obtain high-performance composite modified petroleum coke.

[0009] The mass ratio of the calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride and sodium silicate for stirring is: 80~83:7~10:3.5~4:3~4.5:3~3.5:1~2; a paddle-type stirring paddle is used, the stirring speed is 100~200 rpm, the power is set to 5~15 kW, and the stirring time is 20 minutes.

[0010] The intercalation reaction is carried out for 2 to 4 hours at a temperature of 500 to 600°C.

[0011] The process of mapping all temperature difference samples and combining them with anomaly detection to obtain segmented samples includes:

[0012] Calculate the mean and variance of all data in each temperature difference sample as the horizontal and vertical coordinates in the two-dimensional coordinate system respectively;

[0013] All data points in the coordinate system are detected using anomaly detection to obtain outliers, and the temperature difference samples corresponding to the outliers are used as segmentation samples.

[0014] The temperature control process of the sintering furnace is divided based on the segmented samples, and the temperature difference matrix of each divided interval is determined in combination with the temperature difference samples corresponding to the divided intervals, specifically:

[0015] The acquisition time corresponding to the segmented sample is used as the segmentation time, and the time interval corresponding to all temperature difference samples is divided to obtain several segmentation intervals;

[0016] The matrix composed of temperature difference samples in the same divided interval is used as the temperature difference matrix corresponding to each divided interval.

[0017] The comparison of responses of different batches to temperature control in the temperature difference matrix and the data change trend of the temperature difference matrix are combined to obtain the response difference value of each batch, including:

[0018] The temperature difference matrix of each divided interval is used as input, and the objective weighting method is used to obtain the weight corresponding to each row of data in the temperature difference matrix;

[0019] Calculate the absolute value of the difference between the weight corresponding to the temperature difference data of each batch in the temperature difference matrix and the weight corresponding to the temperature difference data of other batches, and take the mean of all the absolute values as the consistency difference of each batch;

[0020] Analyze the trend statistics of each batch in each temperature difference matrix, obtain the average level of the trend statistics of each batch in all temperature difference matrices and the consistency difference for forward fusion, and obtain the response difference value of each batch.

[0021] The parameters of the sintering furnace temperature control of the current batch are adjusted according to the response difference value of the previous batch of the current batch, specifically:

[0022] Obtain the normalized result of all response difference values of the previous batch of the current batch. If the normalized result is greater than the preset judgment threshold, adjust the control parameters of the sintering furnace of the current batch. The adjustment formula is: ;in, 、 Respectively represent , Sintering furnace control parameters for each batch; Indicates the Normalized results of response difference values of batches;

[0023] Otherwise, the sintering furnace control parameters of the previous batch are used as the sintering furnace control parameters of the current batch.

[0024] Wherein, the rotation speed of the ball milling is 150-250 rpm.

[0025] The base material, water-soluble cellulose ether, sodium silicate and calcium oxide are added and stirred and mixed in a mass ratio of 100:3.5-4:1-2:3-4.5; the stirring speed is 100-200 rpm, and the stirring is carried out for 15-20 minutes.

[0026] In a second aspect, the embodiments of the present application also provide a high-performance composite modified calcined petroleum coke, which is obtained by the high-performance composite modified calcined petroleum coke preparation method.

[0027] In the above scheme, considering the importance of temperature control accuracy in maintaining The activity and diffusion capacity are significantly affected. Once the sintering reaction temperature is uneven, the reaction rates in different areas will be different, which will lead to uneven product intercalation levels, seriously affecting the uniformity of product quality and performance. To address this problem, the present application proposes a high-performance composite modified calcined petroleum coke and its preparation method, which specifically includes the steps of raw material preparation and testing, particle size screening, uniform stirring of the first dry powder mixer, base material preparation, base material crushing, base material particle size screening, second dry powder mixer mixing and stirring, mechanical granulation and quantitative packaging. By introducing an industrial control system, the preparation and production process at each stage is precisely controlled.

[0028] At the same time, in response to the key issue of the impact of sintering parameter control on the performance of petroleum coke during the production process, this application focuses on analyzing the temperature deviation during the preparation of different batches of petroleum coke, as well as the trend characteristics of the temperature deviation during the control process. On this basis, the control parameters in the sintering process are optimized and adjusted to effectively avoid the situation where the degree of product intercalation is different due to uneven sintering reaction temperature, solve the problem of product quality and performance uniformity being affected, and thus significantly improve the preparation and production quality of high-performance composite modified petroleum coke. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 A flowchart of a method for preparing high-performance composite modified calcined petroleum coke provided in one embodiment of the present application;

[0030] Figure 2 A flow chart for controlling temperature parameters during an intercalation reaction is provided for one embodiment of the present application. DETAILED DESCRIPTION

[0031] In the description of the embodiments of this application, words such as "exemplary," "or," and "for example" are used to indicate examples, illustrations, or descriptions. Any embodiment or design described as "exemplary" or "for example" in the embodiments of this application should not be construed as being preferred or advantageous over other embodiments or designs. Rather, the use of words such as "exemplary," "or," and "for example" is intended to present the relevant concepts in a concrete manner.

[0032] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art in the art of this application. The terms used in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application.

[0033] It should also be noted that the terms "first" and "second" in this application and the accompanying drawings are used to distinguish similar objects, rather than to describe a specific order or sequence. The methods disclosed in the embodiments of this application or the methods shown in the flowcharts include one or more steps for implementing the methods. Without departing from the scope of protection of this application, the order of executing multiple steps can be interchanged with each other, and some steps can also be deleted.

[0034] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.

[0035] The specific scheme of a high-performance composite modified calcined petroleum coke and its preparation method provided by the present application is described in detail below with reference to the accompanying drawings.

[0036] Example 1

[0037] See also Figure 1 , which shows a flow chart of the steps of a method for preparing high-performance composite modified calcined petroleum coke provided in Example 1 of the present application, the method comprising the following steps:

[0038] S1, Raw material preparation and testing

[0039] Prepare calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride, and sodium silicate. Use chemical analysis instruments to test the purity and impurity content of each raw material to ensure it meets production requirements. In this application, a spectrometer is used to detect trace elements in the raw materials.

[0040] S2, particle size screening

[0041] The calcined petroleum coke is screened for particle size using a vibrating screen, specifically a 100-200 mesh screen, to remove particles that do not meet the particle size requirements, making it easier to mix evenly in the subsequent stirring.

[0042] S3, the first dry powder mixer is used for uniform mixing

[0043] Calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride, and sodium silicate were added to a dry powder mixer in a mass ratio of 80:7:3.5:3:3:1. The mixer was turned on, set to a speed of 200 rpm and a power of 5 kW, and stirred for 20 minutes using a paddle-type impeller to ensure thorough mixing and effective mixing. During the dry powder mixer's mixing process, a speed sensor was used to collect the mixing speed in real time. This data was then transmitted to an industrial control system, which controlled the mixing speed in real time.

[0044] S4, base material preparation

[0045] The mixture after stirring and mixing is divided evenly and added into the vacuum sintering furnace in batches. The temperature in the furnace is set at conduct Intercalation reaction, the reaction time is 4 hours, the preparation - Graphite intercalation compound; in the above-mentioned process, the temperature data of the reaction process is collected in real time by the temperature sensor provided, and the collected temperature data is transmitted to the industrial control system in real time. The flow chart of the control of the temperature parameters in the intercalation reaction process by the industrial control system is as follows Figure 2 shown.

[0046] The vacuum environment created by the vacuum sintering furnace can effectively prevent the graphite and copper chloride in the mixture from oxidizing at high temperatures, reduce the generation of impurities, and ensure The purity of the graphite intercalation compound is improved, and the volatile impurities in the raw materials are removed to improve the purity and efficiency of the intercalation reaction. The reaction temperature is set at ,at this time It has a certain activity, which can overcome the interlayer force of graphite to complete the intercalation, and will not destroy the graphite structure or cause it to break due to excessive temperature. break down.

[0047] The temperature data is collected in real time by the temperature sensor and transmitted to the industrial control system for regulation to ensure that the reaction temperature is stable. ; The controller for sintering furnace temperature control in the industrial control system is a PID controller, and the initial value of the PID controller parameter is determined by the attenuation curve method.

[0048] During the production and preparation of calcined petroleum coke, the temperature uniformity of the reaction process varies due to the stability of the heating elements in the reactor, which results in differences in the intercalation reaction between different batches. Therefore, when determining the temperature adjustment parameters for the current batch, the differences in the response speed of the temperature control between different batches are fully considered, and the temperature control response parameters in the current industrial system are adjusted. The specific adjustment process is as follows:

[0049] (1) Compare the temperature control deviations of different batches of reaction processes in industrial control systems and obtain segmented samples.

[0050] For each batch of calcined petroleum coke produced up to the current time, obtain the temperature data of each sampling moment in the base material preparation reaction process of each batch, take the difference between each temperature data and the set standard temperature as the temperature difference at the sampling moment, and construct a temperature difference sample by taking the temperature differences of the same sampling moments in the base material preparation reaction process of all batches. , all batches of base material preparation process The temperature difference samples are recorded as ,in, 、 、 The first batch, the second batch, The first step in the batch base material preparation reaction process In this embodiment, the standard temperature is ; Implementers can make adjustments based on actual conditions.

[0051] Data mapping is performed on all temperature difference samples. The mapping method is as follows: the mean and variance of all data in each temperature difference sample are calculated, and the values are used as the horizontal and vertical coordinates in the two-dimensional coordinate system, so that each temperature difference sample is mapped to a data point in the two-dimensional coordinate system. All data points are used as input, and anomaly detection methods are used to detect and obtain anomalies. The temperature difference samples corresponding to the anomalies are used as segmentation samples. Compared with directly performing anomaly detection on temperature difference samples, mapping the mean and variance before performing anomaly detection can accurately compare the control response differences of different batches in the preparation process at different time periods. Among them, commonly used methods for anomaly detection include but are not limited to the local outlier factor algorithm and the DBSCAN algorithm.

[0052] (2) The sintering furnace temperature control process is divided according to the segmented samples, and a deviation comparison analysis is performed based on the division results.

[0053] For the temperature difference samples and segmented samples obtained in the above process, the acquisition time corresponding to the segmented samples is used as the segmentation time, and the time intervals corresponding to all temperature difference samples are divided; specifically, for example, the segmentation time corresponding to the segmented samples is 、 and , if the time interval is [ ],in 、 Represent the 1st and mth acquisition moments respectively; the division intervals are [ 、[ 、[ and[ ]; the temperature difference samples in the same divided interval The matrix formed in the order of acquisition time is used as the temperature difference matrix corresponding to each divided interval; for example, the divided interval [ ]The temperature difference matrix composed of the temperature difference samples corresponding to It should be understood that each row of the temperature difference matrix corresponds to the temperature difference value of the same batch within the corresponding divided interval.

[0054] In order to accurately reflect the differences in temperature control responses of different batches within the divided interval corresponding to each temperature difference matrix, each temperature difference matrix is used as input, and the CRITIC method is used to obtain the weight corresponding to each row of data in the temperature difference matrix. The absolute value of the difference between the weight corresponding to each row of data in the temperature difference matrix and the weight corresponding to each other row of data is calculated, and the average of all the absolute values is taken as the consistency difference of each row of data.

[0055] Based on the consistency difference of each row of data in all divided temperature difference matrices for each batch and the trend characteristics of data changes in each temperature difference matrix, the response difference value of the sintering furnace temperature control in the preparation and production process of each batch is calculated. Specifically, the trend statistics of each batch in each temperature difference matrix are analyzed; the average level of the trend statistics of each batch in all temperature difference matrices is obtained by forward fusion of the consistency difference, and the response difference value of each batch is obtained.

[0056] In this embodiment, the trend statistic is calculated using the trend verification method, which is a well-known technology and will not be described in detail here; the forward fusion of multiple variables is calculated using the multiplication method; the average level is calculated using the averaging method.

[0057] It should be understood that the larger the calculated result of the response difference value, the greater the deviation of the temperature control of the industrial control system at different times during the preparation process, and the greater the response difference of the temperature control in the industrial control system.

[0058] (3) Based on the response difference value of the temperature control in the production process of the previous batch, the parameters of the sintering furnace control in the preparation process of the current batch are optimized and adjusted to obtain the graphite intercalation compound.

[0059] During the production of high-performance composite modified calcined petroleum coke, if no significant difference in temperature control response speed was observed during the previous batch's production, the sintering furnace control parameters for the current batch's production will not be optimized or adjusted; otherwise, the sintering furnace control parameters for the current batch's production will be optimized and adjusted. For example, during the previous batch's production, if the industrial system's temperature control was relatively stable within the set range, and no significant change in the temperature control deviation at the aforementioned different time periods occurred relative to other batches already produced, this indicates that the PID controller for temperature control of the sintering furnace in the industrial control system responded promptly to temperature changes under the set proportional parameters; otherwise, this indicates that the PID controller for temperature control in the industrial control system during the previous batch's production did not respond promptly under the set proportional parameters, resulting in a significant difference in control response.

[0060] Therefore, in this application, the response difference values of the temperature control of all batches are used as input, and the normalization method is used to obtain the normalized results of the response difference values of all the temperature controls. In order to avoid excessive optimization and adjustment during the production process, the judgment threshold for optimization and adjustment is set to 0.2 in this application. If the normalized result of the response difference value of the temperature control of the previous batch is greater than the judgment threshold, the sintering furnace control parameters of the current batch of preparation and production are adjusted. The specific adjustment relationship is: ;in, 、 Respectively represent , The sintering furnace control parameters in the batch production process are proportional parameters in the controller. The larger the adjustment range of the control parameters, the faster the response to temperature fluctuations in the current batch production process is required to maintain temperature stability. Indicates the Normalized results of response difference values of the production process of each batch preparation.

[0061] Based on the above process, for the production of the current batch, if there is no significant difference in the control response speed during the production of the previous batch, it indicates that the temperature sensor in the current production stage can collect temperature data in real time and accurately, and transmit it to the controller in the industrial control system that controls the sintering furnace temperature through an electrical signal. At the same time, the normalized result of the calculated response difference value of the temperature control of the previous batch is less than the judgment threshold, and the control parameters of the controller for temperature control of the previous batch of industrial production system are retained, so that the controller can smoothly adjust the output power of the control signal in the current batch production process; otherwise, the control parameters of the controller are adjusted accordingly to avoid oscillation of the sintering furnace temperature control due to delay or overshoot, which affects the quality of sintering preparation production.

[0062] Precise sintering temperature control during the production of graphite intercalation compounds can better maintain Activity and diffusion capacity are used to ensure that the intercalation reaction proceeds at the expected rate and manner, and to stabilize the product structure and performance. Therefore, the sintering furnace control parameters are adjusted and determined during the preparation and production process of each batch, and the stability of the preparation and production process is maintained through the industrial control system based on the adjusted results, thereby reducing the quality consistency differences of products prepared from different batches and obtaining graphite intercalation compounds.

[0063] S5, base material crushing

[0064] The graphite intercalation compound is crushed in a jaw crusher and then, after initial crushing, pulverized in a ball mill to a particle size of 200 mesh. The ball mill speed is set at 250 rpm. A speed sensor collects real-time data on the ball mill speed and transmits the collected data to an industrial control system in real time, which controls the speed during the base material crushing process.

[0065] S6, base material particle size screening

[0066] The base material after crushing and ball milling is screened through a vibrating screen to ensure that the particle size meets the 200 mesh requirement and remove oversized or undersized particles. The screen is 200 mesh.

[0067] S7, the second dry powder mixer mixing

[0068] Raw material addition: Add the base material, water-soluble cellulose ether, sodium silicate, and calcium oxide to a dry powder blender in a mass ratio of 100:3.5:1:3. Turn on the blender, set the stirring speed to 100 rpm, and stir for 20 minutes to ensure thorough mixing. A speed sensor collects real-time stirring speed data and transmits this data to the industrial control system, which controls the stirring speed in real time.

[0069] S8, mechanical granulation

[0070] The mixed material is passed through a mechanical granulation device to form spherical granules with a diameter of 0.5 to 1.5 mm. The mechanical granulation device uses an extrusion granulator, and the screw speed of the extrusion granulator is set at 30 revolutions per minute. The speed sensor collects real-time data on the screw speed of the extrusion granulator, transmits the collected data in real time to an industrial control system, and the industrial control system controls the screw speed of the extrusion granulator in real time.

[0071] S9, quantitative packaging

[0072] The granulated product is quantitatively weighed by an electronic weighing device and packaged by an automatic packaging machine according to the prescribed packaging specifications to obtain high-performance composite modified calcined petroleum coke; the packaging speed is 10 to 30 packages per minute.

[0073] Example 2

[0074] See also Figure 1, which shows a step flow chart of a method for preparing a high-performance composite modified calcined petroleum coke provided in Example 2 of the present application, the method is consistent with the steps in Example 1; wherein, in S3, calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride and sodium silicate are added to a dry powder mixer in a mass ratio of 83:10:4:4.5:3.5:2, and the stirring speed is set to 200 rpm and the power is set to 15 kW; in S4, the reaction time in the furnace is 3 hours; in S5, the ball mill speed is set to 250 rpm; in S7, the base material, water-soluble cellulose ether, sodium silicate and calcium oxide are added to the dry powder mixer in a mass ratio of 100:4:2:4.5. The mixer is turned on, the stirring speed is set to 200 rpm, and the stirring is carried out for 15 minutes; in S8, the screw speed of the extrusion granulator is set to 60 rpm.

[0075] Example 3

[0076] See also Figure 1 , which shows a step flow chart of a method for preparing a high-performance composite modified calcined petroleum coke provided in Example 3 of the present application, the method is consistent with the steps in Example 1; wherein, in S3, calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride and sodium silicate are added to a dry powder mixer in a mass ratio of 80:10:3.5:4:3.5:1, and the stirring speed is set to 200 rpm and the power is set to 5 kW; in S4, the reaction time in the furnace is 2 hours; in S5, the ball mill speed is set to 150 rpm; in S7, the base material, water-soluble cellulose ether, sodium silicate and calcium oxide are added to the dry powder mixer in a mass ratio of 100:3.5:1:4. The mixer is turned on, the stirring speed is set to 100 rpm, and the stirring is carried out for 20 minutes; in S8, the screw speed of the extrusion granulator is set to 45 rpm.

[0077] Specifically, a comparison of the parameters of the calcined petroleum coke obtained in the present application and the petroleum coke produced by the traditional method in terms of bulk resistivity, impulse current tolerance and power frequency current tolerance is shown in the following table, wherein Example 1 and Example 2 adopt the preparation method in the present application, and Comparative Example 1 and Comparative Example 2 do not adopt the method for optimizing the production process control, but the specific implementation process and parameters are: Example 1 is the same as Comparative Example 1, and Example 2 is the same as Comparative Example 2.

[0078] Table 1: Calcined petroleum coke parameter comparison table

[0079]

[0080] Among them, the conventional test range of impulse current is 10~50KA, and the conventional test range of power frequency current is 1~10KA. Indicates the resistance difference before and after impact.

[0081] Through the analysis of the test data in the table, it can be seen that after the optimization and adjustment of the production process, the petroleum coke produced by Example 1 and Example 2 shows better performance. Compared with Comparative Examples 1 and 2, the petroleum coke produced by Example 1 and Example 2 has lower bulk resistivity; at the same time, in the impulse current tolerance and power frequency current tolerance tests, the resistance change of the petroleum coke of Example 1 and Example 2 is significantly smaller; this means that the resistance change of petroleum coke under current impulse or power frequency current is small, it has good conductivity and strong impact resistance, and can effectively withstand current fluctuations without significant resistance changes. The differences in these performance parameters fully demonstrate that the preparation method of the present application can effectively improve the quality characteristics of petroleum coke reflected in bulk resistivity, impulse current tolerance and power frequency current tolerance, and significantly improve product performance.

[0082] Based on the same inventive concept as the above method, the embodiment of the present application also provides a high-performance composite modified calcined petroleum coke, which is obtained by the high-performance composite modified calcined petroleum coke preparation method.

[0083] In summary, the embodiment of the present application takes into account the importance of temperature control accuracy in maintaining The activity and diffusion capacity are significantly affected. Once the sintering reaction temperature is uneven, the reaction rates in different areas will be different, which will lead to uneven product intercalation levels, seriously affecting the uniformity of product quality and performance. To address this problem, the present application proposes a high-performance composite modified calcined petroleum coke and its preparation method, which specifically includes the steps of raw material preparation and testing, particle size screening, uniform stirring of the first dry powder mixer, base material preparation, base material crushing, base material particle size screening, second dry powder mixer mixing and stirring, mechanical granulation and quantitative packaging. By introducing an industrial control system, the preparation and production process at each stage is precisely controlled.

[0084] At the same time, in response to the key issue of the impact of sintering parameter control on the performance of petroleum coke during the production process, this application focuses on analyzing the temperature deviation during the preparation of different batches of petroleum coke, as well as the trend characteristics of the temperature deviation during the control process. On this basis, the control parameters in the sintering process are optimized and adjusted to effectively avoid the situation where the degree of product intercalation is different due to uneven sintering reaction temperature, solve the problem of product quality and performance uniformity being affected, and thus significantly improve the preparation and production quality of high-performance composite modified petroleum coke.

[0085] The flowcharts and block diagrams in the accompanying drawings show the possible architecture, functions and operations of the systems, methods and computer program products according to the embodiments of the present application. In this regard, each box in the flowchart or block diagram can represent a module, a program segment or a part of the code, and the part of the module, program segment or code contains one or more executable instructions for realizing the specified logical function. In some alternative implementations, the functions marked in the box can also occur in an order different from that marked in the accompanying drawings. For example, two consecutive boxes can actually be executed substantially in parallel, and they can sometimes be executed in the opposite order, which can depend on the functions involved. In the description corresponding to the flowcharts and block diagrams in the accompanying drawings, the operations or steps corresponding to different boxes can also occur in an order different from that disclosed in the description, and sometimes there is no specific order between different operations or steps. For example, two consecutive operations or steps can actually be executed substantially in parallel, and they can sometimes be executed in the opposite order, which can depend on the functions involved. Each block in the block diagrams and / or flowcharts, and combinations of blocks in the block diagrams and / or flowcharts, may be implemented by a dedicated hardware-based system that performs the specified function or action, or may be implemented by a combination of dedicated hardware and computer instructions.

[0086] It is obvious to those skilled in the art that the present application is not limited to the details of the above exemplary embodiments, and that the present application can be implemented in other specific forms without departing from the basic features of the present application. Therefore, from any point of view, the above embodiments of the present application should be regarded as exemplary and non-restrictive; modifications to the technical solutions described in the above embodiments, or equivalent replacement of some of the technical features therein, do not deviate from the essence of the corresponding technical solutions within the scope of the technical solutions of the embodiments of the present application, and should be included in the scope of protection of the present application.

Claims

1. A method for preparing high-performance composite modified calcined petroleum coke, characterized in that: The method comprises the following steps: Calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride and sodium silicate are mixed and stirred, and the stirred mixture is placed in batches into a sintering furnace for intercalation reaction. The temperature difference between temperature data at each acquisition moment and preset temperature data is obtained, and all the temperature differences in the same order of all batches are combined into a temperature difference sample. The mean and variance of all data in each temperature difference sample are calculated and used as the horizontal and vertical coordinates in a two-dimensional coordinate system, respectively; all data points in the coordinate system are detected by anomaly detection to obtain abnormal points, and the temperature difference samples corresponding to the abnormal points are used as segmentation samples; The acquisition time corresponding to the segmented sample is used as the segmentation time, and the time interval corresponding to all temperature difference samples is divided to obtain several segmented intervals; the matrix composed of the temperature difference samples in the same segmented interval is used as the temperature difference matrix corresponding to each segmented interval; the temperature difference matrix of each segmented interval is used as input, and the objective weighting method is used to obtain the weight corresponding to each row of data in the temperature difference matrix; the absolute value of the difference between the weight corresponding to each batch of temperature difference data in the temperature difference matrix and the weight corresponding to other batches is calculated, and the mean of all the absolute values is used as the consistency difference of each batch; the trend statistics of each batch in each temperature difference matrix are analyzed, and the average level of the trend statistics and consistency differences of each batch in all temperature difference matrices are forward fused to obtain the response difference value of each batch; the normalized result of all response difference values of the previous batch of the current batch is obtained. If the normalized result is greater than the preset judgment threshold, the sintering furnace control parameters of the current batch are adjusted. The adjustment formula is: ;in, 、 Respectively represent , Sintering furnace control parameters for each batch; Indicates the The normalized result of the response difference value of each batch is obtained; otherwise, the sintering furnace control parameters of the previous batch are used as the sintering furnace control parameters of the current batch; wherein, the initial value of the sintering furnace control parameter is determined by the decay curve method; After the graphite intercalation compound is crushed by ball milling, base material, water-soluble cellulose ether, sodium silicate and calcium oxide are added and stirred and mixed continuously. The mixed materials are mechanically granulated and packaged to obtain high-performance composite modified petroleum coke.

2. The method for preparing high-performance composite modified calcined petroleum coke according to claim 1, wherein: The mass ratio of the calcined petroleum coke, flake graphite powder, water-soluble cellulose ether, calcium oxide, copper chloride and sodium silicate for stirring is 80-83:7-10:3.5-4:3-4.5:3-3.5:1-2; a paddle-type stirring paddle is used, the stirring speed is 100-200 rpm, the power is set to 5-15 kW, and the stirring time is 20 minutes.

3. The method for preparing high-performance composite modified calcined petroleum coke according to claim 1, wherein: The intercalation reaction is carried out for 2 to 4 hours at a temperature of 500 to 600°C.

4. The method for preparing high-performance composite modified calcined petroleum coke according to claim 1, wherein: The rotation speed of the ball milling is 150 to 250 revolutions per minute.

5. The method for preparing high-performance composite modified calcined petroleum coke according to claim 1, wherein: The base material, water-soluble cellulose ether, sodium silicate and calcium oxide are added and stirred and mixed in a mass ratio of 100:3.5-4:1-2:3-4.5; the stirring speed is 100-200 rpm, and the stirring is carried out for 15-20 minutes.

6. A high-performance composite modified calcined petroleum coke, characterized in that: The high-performance composite modified calcined petroleum coke is obtained by the preparation method according to any one of claims 1 to 5.

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