CN118221447A - Preparation method of special heat preservation material for isostatic pressure graphite - Google Patents

Preparation method of special heat preservation material for isostatic pressure graphite Download PDF

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CN118221447A
CN118221447A CN202410635181.9A CN202410635181A CN118221447A CN 118221447 A CN118221447 A CN 118221447A CN 202410635181 A CN202410635181 A CN 202410635181A CN 118221447 A CN118221447 A CN 118221447A
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temperature
heat flow
pixel
calcining
pixels
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CN118221447B (en
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刘京龙
李晨曦
李重阳
李博文
李�浩
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Panjin Youbang Tes Trading Co ltd
Panjin Jiatan New Material Co ltd
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Panjin Youbang Tes Trading Co ltd
Panjin Jiatan New Material Co ltd
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Abstract

The invention relates to the technical field of calcined petroleum coke preparation, in particular to a preparation method of an isostatic pressing graphite special heat preservation material, which comprises the following steps: the method comprises the steps of crushing and drying petroleum coke, putting the petroleum coke into microwaves for irradiation, uniformly mixing the irradiated petroleum coke with a composite extractant, then connecting a recovery condensing device and a stirring device, reacting for 1.5 hours at 150 ℃, then carrying out suction filtration, washing and drying to obtain primary treated petroleum coke, uniformly mixing the primary treated petroleum coke with manganese powder and paraffin according to a proportion to obtain a mixture, calcining the mixture in a calciner, collecting infrared thermal imaging images in the calcining process, obtaining calcining sufficiency of the infrared thermal imaging images at each moment according to the temperature distribution characteristics of the infrared thermal imaging images, and adjusting the calcining time. The invention aims to ensure that the petroleum coke mixture is fully calcined and improve the desulfurization rate of petroleum coke.

Description

Preparation method of special heat preservation material for isostatic pressure graphite
Technical Field
The invention relates to the technical field of calcined petroleum coke preparation, in particular to a preparation method of an isostatic pressing graphite special heat preservation material.
Background
The special heat-insulating material for the isostatic pressing graphite is a heat-insulating material for producing high-purity, high-precision and high-hardness isostatic pressing graphite grinding tools or materials, and can effectively keep the temperature stable in the production process, reduce heat loss or excessive diffusion, thereby improving the production efficiency and the product quality. The calcined petroleum coke with high carbon content, low volatility, high density and good heat preservation performance is an ideal choice of heat preservation materials of the graphitization furnace in the production process of the isostatic pressing graphite, and is beneficial to producing the high-quality isostatic pressing graphite.
In the preparation process of the isostatic pressing graphite special heat preservation material, namely the calcined petroleum coke, the calcination time of the petroleum coke control mixture needs to be strictly controlled, and excessive graphitization or structural damage of the petroleum coke can be caused by the overlong calcination time, so that the heat preservation and heat resistance are reduced, and the stability and durability of the isostatic pressing graphite heat preservation material are affected; too short a calcination period may result in insufficient desulfurization and graphitization of the petroleum coke, failing to achieve the desired density and strength of the petroleum coke, affecting the service life in high temperature environments.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a special heat preservation material for isostatic pressing graphite, which aims to solve the existing problems.
The preparation method of the special heat preservation material for the isostatic pressing graphite adopts the following technical scheme:
the embodiment of the invention provides a preparation method of an isostatic pressing graphite special heat preservation material, which comprises the following steps:
(1) Pulverizing and drying petroleum coke, and then placing the petroleum coke into microwaves for irradiation;
(2) Uniformly mixing the petroleum coke irradiated in the step (1) with a composite extractant, connecting a recovery condensing device and a stirring device, and reacting for 1.5 hours at 150 ℃;
(3) Processing the petroleum coke prepared in the step (2) to obtain primary processed petroleum coke;
(4) Uniformly mixing the primary treated petroleum coke in the step (3) with manganese powder and paraffin according to a proportion to obtain a mixture;
(5) Calcining the mixture obtained in the step (4) in a calciner for 1-1.5 h, and collecting infrared thermal imaging images of the mixture at each moment after calcining for 1 h; uniformly and symmetrically dividing the infrared thermal imaging image at each moment into two calcining areas; acquiring a preset pixel window of each pixel by taking each pixel in the infrared thermal imaging image as a center; obtaining high-temperature significant pixels, low-temperature significant pixels and heat flow paths and heat flow sequences corresponding to the high-temperature significant pixels of each pixel window according to the temperature distribution characteristics of the pixels in the infrared thermal imaging image at each moment; obtaining the heat flow fully uniform coefficient of each pixel window in the infrared thermal imaging image at each moment according to the distribution of the heat flow paths and the heat flow sequences corresponding to the high-temperature significant pixel, the low-temperature significant pixel and the high-temperature significant pixel; obtaining calcining sufficiency of the infrared thermal imaging image at each moment according to the distribution of the heat flow sufficient uniformity coefficient of each pixel window in the two calcining areas; and (3) adjusting the calcination time of the mixture in the calciner according to the calcination sufficiency of the infrared thermal imaging image at each moment, and preparing the special heat-insulating material for the isostatic pressing graphite after completing calcination.
Preferably, the step of pulverizing and drying petroleum coke and then placing the petroleum coke into microwaves for irradiation comprises the following steps:
the petroleum coke is crushed and sieved by a 10-mesh sieve, then is dried for 12 hours at 200 ℃ by a petroleum coke dryer, and is then put into microwaves to be irradiated for 30 minutes under the power of 450W.
Preferably, the step (1) of uniformly mixing the petroleum coke irradiated by the step (1) with the composite extractant comprises the following steps:
The composite extractant is prepared by mixing o-chlorophenol and furfural in a volume ratio of 2:1, and the liquid-solid ratio of the composite extractant to petroleum coke is 12:1.
Preferably, the step (2) of processing the petroleum coke to obtain the primary processed petroleum coke includes:
And (3) carrying out suction filtration, washing and drying on the petroleum coke prepared in the step (2) to obtain the primary treatment petroleum coke.
Preferably, the petroleum coke, the manganese powder and the paraffin are uniformly mixed according to the proportion, wherein the mass ratio of the petroleum coke to the manganese powder to the paraffin is 10:1:1.
Preferably, the calcination temperature of the calcination in the calciner is 700 ℃.
Preferably, the heat flow path and the heat flow sequence corresponding to the high-temperature significant pixel, the low-temperature significant pixel and the high-temperature significant pixel of each pixel window include:
For pixel windows of all pixels, ascending temperature values of all pixels in the pixel windows are arranged to be used as window temperature sequences of the pixels, a first quartile and a third quartile of the window temperature sequences are calculated, the pixel temperature ascending sequences with the temperature values smaller than or equal to the first quartile in the pixel windows are used as window first temperature sequences of the pixels, the pixel temperature ascending sequences with the temperature values larger than or equal to the third quartile in the pixel windows are used as window third temperature sequences of the pixels, an OTSU (open-close method) is utilized to respectively obtain a window first temperature sequence of the pixels and a segmentation threshold value of the window third temperature sequence, pixels with the temperature values smaller than or equal to the segmentation threshold value in the window first temperature sequence are used as low-temperature significant pixels of the pixels, and pixels with the temperature values larger than or equal to the segmentation threshold value in the window third temperature sequence are used as high-temperature significant pixels of the pixels;
And taking the connection line from each high-temperature obvious pixel to each low-temperature obvious pixel in the pixel window of each pixel as a heat flow path of each high-temperature obvious pixel, and taking the temperature values of all pixels on the heat flow path of each high-temperature obvious pixel as a heat flow sequence corresponding to the heat flow path.
Preferably, the heat flow coefficient of each pixel window in the infrared thermal imaging image at each moment is sufficiently uniform, including:
calculating the ratio of the total number of high-temperature significant pixels to the total number of low-temperature significant pixels according to pixel windows of all pixels, calculating the difference value of the temperature value of all low-temperature significant pixels and the temperature minimum value of all low-temperature significant pixels, calculating the sum value of the difference values of all low-temperature significant pixels, marking the sum value as a first sum value, calculating the difference value of the temperature maximum value of all high-temperature significant pixels and the temperature value of all high-temperature significant pixels, marking the sum value as a first difference value, calculating the sum value of the first difference value of all high-temperature significant pixels as a second sum value, calculating the sum result of the second sum value and an adjustment parameter which is preset to be larger than 0, calculating the ratio of the first sum value and the sum result, and taking the product of the two ratios as a heating sufficient factor of each pixel window;
Heat flow uniformity factor of jth high-temperature significant pixel in ith pixel window at t moment The expression of (2) is:
In the method, in the process of the invention, The total number of heat flow paths of the jth high-temperature obvious pixels in the ith pixel window at the t moment,、/>The heat flow sequences corresponding to the kth and z heat flow paths of the jth high-temperature obvious pixel in the ith pixel window at the t moment are respectively/>At dtw distance,/>Is a shannon entropy function,/>Is a natural constant,/>Adjusting parameters for presetting to be larger than 0;
Taking a normalized value of a product of a heating sufficient factor of each pixel window in the infrared thermal imaging image at each moment and a sum value of heat flow uniformity factors of all high-temperature obvious pixels in the pixel windows as a heat flow sufficient uniformity coefficient of each pixel window in the infrared thermal imaging image at each moment.
Preferably, the obtaining the calcining sufficiency of the infrared thermal imaging image at each moment according to the distribution of the heat flow sufficient uniformity coefficient of each pixel window in two calcining areas includes:
Giving the heat flow fully uniform coefficient of each pixel window in the infrared thermal imaging image at each moment to the central pixel of the corresponding pixel window to obtain the heat flow fully uniform coefficient of each pixel in the infrared thermal imaging image at each moment, and marking a calcining area close to the burner position of the calcining furnace as a calcining area The other calcination zone is denoted as calcination zone/>Calcination zone/>The heat flow sufficient uniformity coefficient of all pixels in the inner is used as the input of a clustering algorithm, the output is each heat flow cluster, the heat flow sufficient uniformity coefficient of all pixels in each heat flow cluster is arranged in an ascending order to be used as the heat flow characteristic sequence of each heat flow cluster, and the heat flow characteristic sequence is in a calcining area/>The method comprises the steps of obtaining mirror image clusters symmetrical to each heat flux cluster, arranging heat flux fully uniform coefficients of all pixels in each mirror image cluster in ascending order to serve as mirror image feature sequences of each mirror image cluster, and taking heat flux fully uniform coefficient average values of all pixels in each heat flux cluster as heat flux feature values of each heat flux cluster;
Calcination zone at time t Calcining sufficiency factor/>, of inner p-th thermal clusterThe expression of (2) is:
In the method, in the process of the invention, For the time t calcination zone/>Total number of pixels in inner p-th thermal cluster,/>、/>Calcination zone at time t/>, respectivelyThe heat flow of the q-th pixel in the inner p-th heat flow cluster is fully uniform in coefficient, and the heat flow characteristic value of the p-th heat flow cluster,/>For the time t calcination zone/>Heat flow characteristic value average value of all heat flow clusters in the reactor,/>For presetting the adjustment parameter larger than 0,/>Is a natural constant; by and calcine zone/>The calcining area/>, obtained by the same calculation method of calcining full factors of all the hot clusters in the reactorCalcining the full factors of each mirror image cluster;
Calcination zone at time t Heat transfer symmetry factor/>, of inner p-th heat clusterThe expression of (2) is:
In the method, in the process of the invention, 、/>Calcination zone at time t/>, respectivelyCalcining sufficiency factor of inner p-th thermal cluster, calcining sufficiency factor of mirror image cluster of p-th thermal cluster,/>For the time t calcination zone/>Total number of hot clusters in/(、/>Calcination zone at time t/>, respectivelyThe heat flow characteristic sequence of the inner p-th heat flow cluster, the mirror image characteristic sequence of the mirror image cluster of the p-th heat flow cluster,/>At dtw distance,/>Presetting an adjustment parameter larger than 0;
calcining the zone at each moment The normalized value of the heat transfer symmetry factor mean value of all the heat clusters in the furnace is used as the calcining sufficiency of the infrared thermal imaging image at each moment.
Preferably, the adjusting the calcining time of the mixture in the calciner according to the calcining sufficiency of the infrared thermal imaging image at each moment includes:
And calculating the calcining sufficiency of the infrared thermal imaging image at each moment, and if the calcining sufficiency is smaller than a preset calcining sufficiency threshold, prolonging the calcining time for 1min until the calcining sufficiency is greater than or equal to the preset calcining sufficiency threshold or the calcining time length reaches 1.5h.
The invention has at least the following beneficial effects:
according to the invention, the heat flow full uniformity coefficient of each pixel is obtained through the temperature distribution characteristics of the pixels in the calcined image, and the analysis of heat flow transmission uniformity is added on the basis of considering the high and low temperature difference in the pixel window, so that the possibility of full and uniform calcination of the petroleum coke mixture at the corresponding position of the pixel window can be reflected more accurately; the method comprises the steps of obtaining each heat flux cluster and mirror image clusters in a calcination area through a heat flux full uniformity coefficient and a clustering algorithm, obtaining calcination sufficiency of a calcination image according to heat flux full uniformity coefficient difference characteristics of pixels in the heat flux clusters and the mirror image clusters, comprehensively considering heat flux full uniformity coefficient change characteristics and symmetry of heat flux transmission, and reflecting calcination sufficiency of petroleum coke mixture more accurately; the calcining time length of the petroleum coke mixture is adaptively adjusted according to the calcining sufficiency of the calcining image, so that the fully desulfurized and calcined petroleum coke is obtained, the defects of excessive graphitization and insufficient desulfurization of the petroleum coke are avoided, and the thermal insulation and heat resistance are better.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions and advantages of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are only some embodiments of the invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of steps of a method for preparing an isostatic pressing graphite special-purpose insulation material according to an embodiment of the invention;
FIG. 2 is a flow chart of calcined petroleum coke production;
FIG. 3 is a schematic view showing the division of the calcining zone of the calciner.
Detailed Description
In order to further illustrate the technical means and effects adopted by the invention to achieve the preset aim, the following is a detailed description of specific implementation, structure, characteristics and effects of the preparation method of the special heat preservation material for isostatic pressing graphite according to the invention in combination with the accompanying drawings and the preferred embodiment. In the following description, different "one embodiment" or "another embodiment" means that the embodiments are not necessarily the same. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
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 invention belongs.
The specific scheme of the preparation method of the special heat preservation material for the isostatic pressing graphite provided by the invention is specifically described below with reference to the accompanying drawings.
Example 1
Embodiment 1 provides a preparation method of an isostatic pressing graphite special-purpose insulation material, the preparation flow chart is shown in fig. 1, and the specific preparation process is as follows:
(1) Crushing and drying: crushing petroleum coke, sieving with a 10-mesh sieve, drying at 200 ℃ for 12 hours by using a petroleum coke dryer, and then placing the crushed and dried petroleum coke into microwaves to irradiate for 30 minutes under 450W power, wherein the irradiation aims to enable chemical bonds in the petroleum coke to vibrate, break and collide with molecular particles by mutual friction, improve the performance of the petroleum coke and improve the desulfurization effect of the subsequent petroleum coke;
(2) And (3) composite extraction: after evenly mixing the irradiated petroleum coke and a composite extractant, connecting a recovery condensing device and a stirring device, and reacting for 1.5 hours at 150 ℃, wherein the composite extractant used in the embodiment is prepared by mixing o-chlorophenol and furfural in a volume ratio of 2:1, and the liquid-solid ratio of the composite extractant to the petroleum coke is 12:1;
(3) Primary treatment: carrying out suction filtration, washing and drying on the petroleum coke subjected to the step (2) to obtain primary treatment petroleum coke;
(4) Mixing materials: uniformly mixing the obtained primary treated petroleum coke with manganese powder and paraffin in a mass ratio of 10:1:1 to obtain a mixture;
(5) Calcining: and (3) placing the mixture into a calciner to calcine for 1-1.5 h at 700 ℃ to obtain the calcined petroleum coke with sufficient desulfurization.
And S001, collecting an infrared thermal imaging image of the mixture in the calcining process of the step (5), and preprocessing.
The infrared thermal imaging image in the petroleum coke mixture calcining process is acquired by an endoscopic in-furnace high-temperature infrared thermal imager, and the acquisition mode is as follows: the collecting is started after the petroleum coke mixture is calcined for 1h, the collecting angle is the overlooking angle, the collecting time interval is 1min, in order to prevent the infrared thermal imaging image in the petroleum coke mixture calcining process from being affected by stronger noise interference, the embodiment uses a bilateral filtering algorithm to carry out denoising treatment on the infrared thermal imaging image in the petroleum coke mixture calcining process obtained by collecting, aims to remove noise and keep detailed information in the image as much as possible, and an operator can select other algorithms to preprocess the infrared thermal imaging image in the petroleum coke mixture calcining process according to actual conditions.
So far, the infrared thermal imaging image in the petroleum coke mixture calcining process based on the time sequence can be obtained, and the infrared thermal imaging image in the petroleum coke mixture calcining process is recorded as a calcining image for convenience of subsequent description.
Step S002, obtaining the heat flow sufficient uniformity coefficient of each pixel through the high and low temperature characteristics and the temperature distribution characteristics of the pixels in the calcined image, obtaining each heat flow cluster and mirror image cluster in the calcined area through the heat flow sufficient uniformity coefficient and the clustering algorithm, and obtaining the calcining sufficiency of the calcined image according to the heat flow sufficient uniformity coefficient difference characteristics of the pixels in the heat flow clusters and the mirror image clusters.
Specifically, in this embodiment, after the petroleum coke is crushed and dried, the petroleum coke is put into microwaves for irradiation, after the irradiated petroleum coke is uniformly mixed with a composite extractant, the petroleum coke is connected with a recovery condensing device and a stirring device and reacts for 1.5 hours at 150 ℃, then the primary treated petroleum coke is obtained after suction filtration, washing and drying, the primary treated petroleum coke, manganese powder and paraffin are uniformly mixed according to a proportion to obtain a mixture, the mixture is calcined in a calciner, infrared thermal imaging images in the calcination process are acquired, the calcination sufficiency of the infrared thermal imaging images at each moment is obtained according to the temperature distribution characteristics of the infrared thermal imaging images, the calcination time is adjusted, and a preparation flow chart of the calcined petroleum coke is shown in fig. 2. The construction process of calcining sufficiency of the infrared thermal imaging image at each moment comprises the following steps:
In the process of calcining the petroleum coke mixture, the more complete the calcining reaction of the petroleum coke mixture, the more uniform the heat distribution in a calcining image, and the higher the temperature value in the petroleum coke mixture area which is fully calcined is obtained, and the lower the temperature value and the non-uniform temperature distribution characteristic in the petroleum coke mixture area which is not fully calcined are obtained; secondly, when the calcination reaction of the petroleum coke mixture is more sufficient, the heat flow transmission path in the petroleum coke mixture region, that is, the temperature value on the path from high to low changes more uniformly, and the symmetry of heat flow transmission is more remarkable.
First, the division of the calciner along the central axis into two mutually symmetrical calcination zones is denoted as、/>Calcination zoneAnd/>Are mirror image areas, will calcine the area/>、/>The nth pair of pixels with central axis symmetry is recorded as the nth pair of mirror image pixels, and the calcining area/>, in the image is calcined at the t momentThe ith pixel in the material is taken as an example for subsequent analysis, the calciner comprises a heat preservation material and the like, and the calcination area division schematic diagram of the calciner is shown in figure 3.
Constructing a pixel window by taking the ith pixel as a center, wherein the size of the pixel window is 9 multiplied by 9, and recording a sequence formed by temperature values of all pixels in the ith pixel window according to ascending order as a window temperature sequence of the ith pixelCalculation/>The first and third quartiles of (a) are respectively denoted as/>All temperature values in the ith pixel window are smaller than or equal to/>The pixel of the (i) pixel is marked as a first pixel of a window of the (i) pixel, and all temperature values in the window of the (i) pixel are larger than or equal to/>The pixel of the (i) pixel is marked as a window third pixel of the (i) pixel, sequences formed by all window first pixel temperature values and all window third pixel temperature values in the (i) pixel window according to ascending order are respectively marked as a window first temperature sequence and a window third temperature sequence of the (i) pixel, and the segmentation threshold values of the window first temperature sequence and the window third temperature sequence of the (i) pixel are respectively marked as/>, wherein the segmentation threshold values of the window first temperature sequence and the window third temperature sequence of the (i) pixel are respectively obtained by an OTSU (optical time series of use) Otsu method、/>The i pixel is smaller than or equal to the first temperature sequence of the corresponding window of the i pixelThe pixel of the (c) is marked as a low-temperature significant pixel of the i-th pixel; the i pixel is larger than or equal to/>, in the third temperature sequence of the window corresponding to the i pixelThe pixel of the (c) is marked as a high-temperature significant pixel of the ith pixel; because the OTSU oxford method is a well-known technique, the specific acquisition process is not described in detail.
The connection line between the jth high-temperature significant pixel and the kth low-temperature significant pixel in the pixel window taking the ith pixel as the center is recorded as the heat flow path of the jth high-temperature significant pixelThe direction of the jth high-temperature significant pixel pointing to the kth low-temperature significant pixel is recorded as a heat flow path/>Heat flow direction of (1) will be the heat flow path/>The sequence of the temperature values of all the pixels according to the sequence of the heat flow direction is recorded as the heat flow sequence/>, of the heat flow path
Based on the analysis, the embodiment constructs a heat flow sufficient uniformity coefficient for representing the degree of sufficient and uniform heat distribution in the petroleum coke mixture calcination process, and the expression is as follows:
In the method, in the process of the invention, Is the heating sufficient factor of the ith pixel window at the t moment,/>、/>Respectively, the total number of high-temperature and low-temperature obvious pixels in the ith pixel window at the t moment,/>、/>The temperature value of the kth low-temperature significant pixel in the ith pixel window at the nth moment and the minimum temperature value in all low-temperature significant pixels in the ith pixel window are respectively/>The maximum temperature value in all high-temperature obvious pixels in the ith pixel window at the t moment and the temperature value of the jth high-temperature obvious pixel in the ith pixel window are respectively calculated as follows,/>For presetting the adjustment parameter larger than 0, the denominator is prevented from being 0, in this embodimentThe practitioner can set himself according to the actual situation, and the embodiment is not limited to this, will/>Marked as first sum,/>Recorded as the first difference,/>Record as the second sum;
heat flow uniformity factor for jth high-temperature significant pixel in ith pixel window at t moment,/> For the total number of heat flow paths of the jth high-temperature obvious pixel in the ith pixel window at the t moment,/>、/>The heat flow sequences corresponding to the kth and z heat flow paths of the jth high-temperature obvious pixel in the ith pixel window at the t moment are respectively/>At dtw distance,/>Is a shannon entropy function,/>Is a natural constant,/>For presetting the adjustment parameter larger than 0, the denominator is prevented from being 0, in this embodiment/>The practitioner can set himself according to the actual situation, and the embodiment is not limited to this;
for the heat flow fully uniform coefficient of the ith pixel window at the t moment,/> Is the heating sufficient factor of the ith pixel window at the t moment,/>For the heat flow uniformity factor of the jth high-temperature significant pixel in the ith pixel window at the t moment, norm () is a normalization function, so that/>The range of values of (2) is between 0, 1.
When the ratio of the total number of high-temperature significant pixels to the total number of low-temperature significant pixels in the ith pixel window is larger, namelyThe larger the number of the high-temperature points is, the more the number of the high-temperature points is in the petroleum coke mixture area at the position corresponding to the ith pixel window is; meanwhile, when the sum of the difference between the temperature values of all low-temperature significant pixels and the minimum temperature value in all low-temperature significant pixels in the ith pixel window is larger, namely/>The larger the difference between the temperature value of all the low-temperature significant pixels in the ith pixel window and the minimum temperature value in the low-temperature significant pixels is larger; at the same time, when the sum of the differences between the maximum temperature value in all high-temperature significant pixels and the temperature values of all high-temperature significant pixels in the ith pixel window is smaller, namely/>The smaller the difference between the temperature value of all high-temperature significant pixels in the ith pixel window and the maximum temperature value in the high-temperature significant pixels is, the more sufficient the calcining reaction of the petroleum coke mixture area at the corresponding position of the ith pixel window is likely to be, and the heating sufficient factor/>The larger.
When the sum of dtw distances between all heat flow paths corresponding to heat flow sequences of the jth high-temperature significant pixel in the ith pixel window is smaller, namelyThe smaller the difference between the temperature conditions of all heat flow paths representing the jth high-temperature significant pixel in the ith pixel window is, the smaller the difference between the temperature conditions of all heat flow paths representing the jth high-temperature significant pixel is; meanwhile, when the sum of shannon entropy of all heat flow paths of the jth high-temperature significant pixel in the ith pixel window is smaller, namely/>, corresponding to the heat flow sequenceThe smaller the temperature value fluctuation degree on all heat flow paths of the jth high-temperature obvious pixel in the ith pixel window is, the more uniform the heat transfer effect is, the heat flow uniformity factor/>, of all heat flow paths of the jth high-temperature obvious pixel in the ith pixel window isThe larger.
When the heating sufficient factor of the ith pixel window at the t moment is larger, namelyThe larger the petroleum coke mixture area calcining reaction at the corresponding position of the ith pixel window is, the more sufficient the calcining reaction is possibly; meanwhile, when the sum of heat flow uniformity factors of all high-temperature obvious pixels in the ith pixel window is larger, namely/>The larger the heat transfer effect on the heat flow path corresponding to all high-temperature obvious pixels in the ith pixel window is, the more uniform the heat transfer effect on the heat flow path corresponding to all high-temperature obvious pixels in the ith pixel window is, the greater the possibility that the petroleum coke mixture at the corresponding position of the ith pixel window is fully and uniformly calcined, and the heat flow is fully uniform by a coefficient/>The larger.
Giving the heat flow fully uniform coefficient of each pixel window to the center pixel in the corresponding pixel window, so as to obtain the calcining region in the calcining image at the t momentThe heat flow of all pixels in the furnace is sufficiently uniform, and the calcining area/>, is adoptedThe calcining area/>, can be obtained by the calculation method that the heat flow of each pixel in the inner pixel is fully uniform and the coefficients are the sameThe heat flow of each pixel in the inner part is uniform. Calcining region/>, in the calcining image at t timeThe heat flow full uniformity coefficients of all the pixels in the petroleum coke mixture are ordered according to ascending order, 10% of the pixels are selected as heat flow characteristic pixels, the more the number of the heat flow characteristic pixels is, the more accurate the subsequent clustering result is, the more accurate the judgment on the calcining full degree of the petroleum coke mixture is, and an implementer can set the number of the heat flow characteristic pixels according to actual conditions.
Calcining zone at t timeThe heat flow sufficient uniformity coefficient of all pixels in the furnace is used as input, and a K-means clustering algorithm is adopted to obtain the calcining region/>All the heat clusters in the reactor, wherein the cluster center is the calcining area/>, at the t momentAnd the absolute value of the difference value of the heat flow fully uniform coefficient between the two pixels is used as a distance measurement mode between the two pixels in the clustering process, and the specific process is not repeated as the K-means clustering algorithm is the prior known technology.
Calcining zone at t timeThe sequence formed by the heat flow fully uniform coefficients of all pixels in the p-th heat flow cluster in the inner heat flow cluster according to the ascending order is used as the heat flow characteristic sequence/>Calcination zone at time t/>The clusters formed by the mirror image pixels of all pixels in the p-th thermal cluster are taken as mirror image clusters of the p-th thermal cluster, and the calcining area/>, at the t-th momentThe sequence formed by the heat flux sufficient uniformity coefficients of all pixels in the mirror image cluster of the p-th heat flux cluster according to the ascending order is recorded as the mirror image characteristic sequence/>Calcination zone at time t/>And (5) the heat flow fully uniform coefficient average value of all pixels in the p-th heat flow cluster in the inner heat flow cluster is recorded as the heat flow characteristic value of the p-th heat flow cluster.
According to the analysis, the embodiment constructs a calcination sufficiency scale for representing the sufficiency degree of the calcination reaction of the petroleum coke mixture, and the expression is:
In the method, in the process of the invention, For the time t calcination zone/>Calcining sufficiency factor of inner p-th heat flux,/>For the time t calcination zone/>Total number of pixels in inner p-th thermal cluster,/>、/>Calcination zone at time t/>, respectivelyThe heat flow of the q-th pixel in the inner p-th heat flow cluster is fully uniform in coefficient, and the heat flow characteristic value of the p-th heat flow cluster,/>For the time t calcination zone/>Heat flow characteristic value average value of all heat flow clusters in the reactor,/>For presetting the adjustment parameters larger than 0, the denominator is prevented from being 0, in this embodiment/>The implementer can set according to the actual situation, and the embodiment does not limit the above, i.e./>Is a natural constant; by and calcine zone/>The calcining area/>, obtained by the same calculation method of calcining full factors of all the hot clusters in the reactorCalcining the full factors of each mirror image cluster;
For the time t calcination zone/> Heat transfer symmetry factor of inner p-th heat cluster,/>、/>Calcination zone at time t/>, respectivelyCalcining sufficiency factor of inner p-th thermal cluster, calcining sufficiency factor of mirror image cluster of p-th thermal cluster,/>For the time t calcination zone/>Total number of hot clusters in/(、/>Calcination zone at time t/>, respectivelyThe heat flow characteristic sequence of the inner p-th heat flow cluster, the mirror image characteristic sequence of the mirror image cluster of the p-th heat flow cluster,/>A dtw distance; /(I)For presetting the adjustment parameter larger than 0, the denominator is prevented from being 0, in this embodiment/>The practitioner can set himself according to the actual situation, and the embodiment is not limited to this;
for the calcination sufficiency of the calcination image at time t,/> For the time t calcination zone/>The total number of hot clusters in the reactor, norm () is a normalization function, so that/>The value range of (2) is in the range of [0,1 ].
Calcining zone at time tThe smaller the sum of the absolute value of the difference between the heat flux coefficient of all pixels in the p-th heat flux and the heat flux characteristic value of the p-th heat flux, namely/>The smaller the difference between the heat flow fully uniform coefficients of all pixels in the p-th heat flux cluster is, the smaller the difference is; at the same time when the t-th time calcines the region/>Heat flow characteristic value of inner p-th heat flow cluster and calcining area/>The larger the difference between the heat flow characteristic value mean values of all the heat flow clusters, namely/>The larger the heat flux of all pixels in the p-th heat flux cluster is, the more uniform the coefficient-to-average ratio of the heat flux isThe larger the average value of the heat flow full uniformity coefficients of all pixels in all the inner heat flow clusters is, the larger the possibility that the petroleum coke mixture at the corresponding position of the p-th heat flow cluster is fully and uniformly calcined is, and the calcining full factor/>The larger.
Calcining zone at time tThe smaller the absolute value of the difference between the calcining sufficiency factor of the inner p-th thermal cluster and the calcining sufficiency factor of the corresponding mirror image cluster, i.e. >The smaller the difference between the calcining fully uniform degree of the petroleum coke mixture at the position corresponding to the p-th thermal cluster and the mirror image cluster is, the smaller the difference is; at the same time when the t-th time calcines the region/>The smaller the dtw distance between the heat flux characteristic sequence of the inner p-th heat flux cluster and the mirror characteristic sequence of the corresponding mirror cluster, namelyThe smaller the difference between the heat flux coefficient of the p-th heat flux cluster and the heat flux coefficient of all pixels in the mirror image cluster is, the stronger the heat flux transfer symmetry at the corresponding position of the p-th heat flux cluster is, and the heat transfer symmetry factor/>The larger.
Calcining zone at time tThe greater the sum of heat transfer symmetry factors for all of the thermal clusters in the reactor, i.eThe larger the calcination area/>, the time t is representedThe higher the calcining degree of the petroleum coke mixture at the corresponding positions of all the hot clusters is, the stronger the symmetry of heat flow transmission is, the more the calcining reaction of the petroleum coke mixture is, and the calcining degree is fullThe higher.
Thus, the calcination sufficiency of the calcination image at each time can be obtained in the above manner.
Step S003, the calcining time length of the petroleum coke mixture is adaptively adjusted according to the calcining sufficiency of the calcining image, the calcining petroleum coke is obtained, and the obtained calcining petroleum coke is tested.
Setting a calcination sufficient threshold H, acquiring the calcination sufficiency of the petroleum coke mixture calcination image in real time, if the calcination sufficiency is smaller than the calcination sufficient threshold H, prolonging the calcination time of the petroleum coke mixture for 1min until the calcination sufficiency of the petroleum coke mixture corresponding to the calcination image is greater than or equal to the calcination sufficient threshold H, or stopping adjusting the calcination time of the petroleum coke mixture when the calcination time of the petroleum coke mixture reaches 1.5H, wherein in the embodiment, the calcination sufficient threshold H=0.8, an implementer can set the calcination sufficient threshold by himself according to actual conditions, the implementation is not limited in this embodiment, and when H is higher, the requirements on the calcination sufficient degree of the petroleum coke mixture are stricter.
According to the preparation method, the calcined petroleum coke with sufficient desulfurization and graphitization can be obtained, and the sulfur content in the raw petroleum coke and the calcined petroleum coke obtained according to the preparation method in the embodiment is respectively measured and recorded as、/>The desulfurization rate calculation results are as follows:
In this example, the sulfur content in the raw petroleum coke was 4.87%, the sulfur content in the calcined petroleum coke obtained by the preparation method in this example was 0.45, and the desulfurization degree calculation result was 90.75%.
In summary, the embodiment of the invention comprehensively considers the characteristic of the heat flow full uniformity coefficient change and the symmetry of heat flow transmission, and more accurately reflects the calcining full degree of the petroleum coke mixture; the calcining time length of the petroleum coke mixture is adaptively adjusted according to the calcining sufficiency of the calcining image, so that the fully desulfurized and calcined petroleum coke is obtained, the defects of excessive graphitization and insufficient desulfurization of the petroleum coke are avoided, and the thermal insulation and heat resistance are better.
It should be noted that: the sequence of the embodiments of the present invention is only for description, and does not represent the advantages and disadvantages of the embodiments. And the foregoing description has been directed to specific embodiments of this specification. In addition, the processes depicted in the accompanying figures do not necessarily require the particular order shown, or sequential order, to achieve desirable results. In some embodiments, multitasking and parallel processing are also possible or may be advantageous.
In this specification, each embodiment is described in a progressive manner, and identical and similar parts of each embodiment are all referred to each other, and each embodiment mainly describes differences from other embodiments.
The foregoing description of the preferred embodiments of the present invention is not intended to be limiting, but rather, any modifications, equivalents, improvements, etc. that fall within the principles of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. The preparation method of the special heat preservation material for the isostatic pressing graphite is characterized by comprising the following steps of:
(1) Pulverizing and drying petroleum coke, and then placing the petroleum coke into microwaves for irradiation;
(2) Uniformly mixing the petroleum coke irradiated in the step (1) with a composite extractant, connecting a recovery condensing device and a stirring device, and reacting for 1.5 hours at 150 ℃;
(3) Processing the petroleum coke prepared in the step (2) to obtain primary processed petroleum coke;
(4) Uniformly mixing the primary treated petroleum coke in the step (3) with manganese powder and paraffin according to a proportion to obtain a mixture;
(5) Calcining the mixture obtained in the step (4) in a calciner for 1-1.5 h, and collecting infrared thermal imaging images of the mixture at each moment after calcining for 1 h; uniformly and symmetrically dividing the infrared thermal imaging image at each moment into two calcining areas; acquiring a preset pixel window of each pixel by taking each pixel in the infrared thermal imaging image as a center; obtaining high-temperature significant pixels, low-temperature significant pixels and heat flow paths and heat flow sequences corresponding to the high-temperature significant pixels of each pixel window according to the temperature distribution characteristics of the pixels in the infrared thermal imaging image at each moment; obtaining the heat flow fully uniform coefficient of each pixel window in the infrared thermal imaging image at each moment according to the distribution of the heat flow paths and the heat flow sequences corresponding to the high-temperature significant pixel, the low-temperature significant pixel and the high-temperature significant pixel; obtaining calcining sufficiency of the infrared thermal imaging image at each moment according to the distribution of the heat flow sufficient uniformity coefficient of each pixel window in the two calcining areas; and (3) adjusting the calcination time of the mixture in the calciner according to the calcination sufficiency of the infrared thermal imaging image at each moment, and preparing the special heat-insulating material for the isostatic pressing graphite after completing calcination.
2. The method for preparing the special heat preservation material for the isostatic pressing graphite, as claimed in claim 1, is characterized in that the method comprises the steps of crushing and drying petroleum coke, and then placing the crushed and dried petroleum coke into microwaves for irradiation, and comprises the following steps:
the petroleum coke is crushed and sieved by a 10-mesh sieve, then is dried for 12 hours at 200 ℃ by a petroleum coke dryer, and is then put into microwaves to be irradiated for 30 minutes under the power of 450W.
3. The method for preparing the special heat preservation material for the isostatic pressing graphite, which is disclosed in claim 1, is characterized in that the method for uniformly mixing the petroleum coke irradiated in the step (1) with the composite extractant comprises the following steps:
The composite extractant is prepared by mixing o-chlorophenol and furfural in a volume ratio of 2:1, and the liquid-solid ratio of the composite extractant to petroleum coke is 12:1.
4. The method for preparing the special heat preservation material for the isostatic pressing graphite, which is disclosed in claim 1, is characterized in that the primary treatment petroleum coke is obtained after the petroleum coke prepared in the step (2) is treated, and comprises the following steps:
And (3) carrying out suction filtration, washing and drying on the petroleum coke prepared in the step (2) to obtain the primary treatment petroleum coke.
5. The preparation method of the special heat preservation material for the isostatic pressing graphite, which is disclosed in claim 1, is characterized in that the evenly mixed petroleum coke, manganese powder and paraffin are mixed according to the mass ratio of 10:1:1.
6. The method for preparing the special heat preservation material for the isostatic pressing graphite as claimed in claim 1, wherein the calcining temperature of the calcination in the calciner is 700 ℃.
7. The method for preparing the special heat preservation material for the isostatic pressing graphite as claimed in claim 1, wherein the heat flow paths and the heat flow sequences corresponding to the high-temperature significant pixels, the low-temperature significant pixels and the high-temperature significant pixels of each pixel window comprise:
For pixel windows of all pixels, ascending temperature values of all pixels in the pixel windows are arranged to be used as window temperature sequences of the pixels, a first quartile and a third quartile of the window temperature sequences are calculated, the pixel temperature ascending sequences with the temperature values smaller than or equal to the first quartile in the pixel windows are used as window first temperature sequences of the pixels, the pixel temperature ascending sequences with the temperature values larger than or equal to the third quartile in the pixel windows are used as window third temperature sequences of the pixels, an OTSU (open-close method) is utilized to respectively obtain a window first temperature sequence of the pixels and a segmentation threshold value of the window third temperature sequence, pixels with the temperature values smaller than or equal to the segmentation threshold value in the window first temperature sequence are used as low-temperature significant pixels of the pixels, and pixels with the temperature values larger than or equal to the segmentation threshold value in the window third temperature sequence are used as high-temperature significant pixels of the pixels;
And taking the connection line from each high-temperature obvious pixel to each low-temperature obvious pixel in the pixel window of each pixel as a heat flow path of each high-temperature obvious pixel, and taking the temperature values of all pixels on the heat flow path of each high-temperature obvious pixel as a heat flow sequence corresponding to the heat flow path.
8. The method for preparing the special heat preservation material for the isostatic pressing graphite as claimed in claim 7, wherein the heat flow of each pixel window in the infrared thermal imaging image at each moment is of a sufficient uniform coefficient, and the method comprises the following steps:
calculating the ratio of the total number of high-temperature significant pixels to the total number of low-temperature significant pixels according to pixel windows of all pixels, calculating the difference value of the temperature value of all low-temperature significant pixels and the temperature minimum value of all low-temperature significant pixels, calculating the sum value of the difference values of all low-temperature significant pixels, marking the sum value as a first sum value, calculating the difference value of the temperature maximum value of all high-temperature significant pixels and the temperature value of all high-temperature significant pixels, marking the sum value as a first difference value, calculating the sum value of the first difference value of all high-temperature significant pixels as a second sum value, calculating the sum result of the second sum value and an adjustment parameter which is preset to be larger than 0, calculating the ratio of the first sum value and the sum result, and taking the product of the two ratios as a heating sufficient factor of each pixel window;
Heat flow uniformity factor of jth high-temperature significant pixel in ith pixel window at t moment The expression of (2) is:
In the method, in the process of the invention, For the total number of heat flow paths of the jth high-temperature obvious pixels in the ith pixel window at the t moment,/>The heat flow sequences corresponding to the kth and z heat flow paths of the jth high-temperature obvious pixel in the ith pixel window at the t moment are respectively/>At dtw distance,/>Is a shannon entropy function,/>Is a natural constant,/>Adjusting parameters for presetting to be larger than 0;
Taking a normalized value of a product of a heating sufficient factor of each pixel window in the infrared thermal imaging image at each moment and a sum value of heat flow uniformity factors of all high-temperature obvious pixels in the pixel windows as a heat flow sufficient uniformity coefficient of each pixel window in the infrared thermal imaging image at each moment.
9. The method for preparing the special heat preservation material for the isostatic pressing graphite as claimed in claim 8, wherein the obtaining of the calcination sufficiency of the infrared thermal imaging image at each moment according to the distribution of the heat flow sufficient uniformity coefficient of each pixel window in the two calcination areas comprises the following steps:
Giving the heat flow fully uniform coefficient of each pixel window in the infrared thermal imaging image at each moment to the central pixel of the corresponding pixel window to obtain the heat flow fully uniform coefficient of each pixel in the infrared thermal imaging image at each moment, and marking a calcining area close to the burner position of the calcining furnace as a calcining area The other calcination zone is denoted as calcination zone/>Calcination zone/>The heat flow sufficient uniformity coefficient of all pixels in the inner is used as the input of a clustering algorithm, the output is each heat flow cluster, the heat flow sufficient uniformity coefficient of all pixels in each heat flow cluster is arranged in an ascending order to be used as the heat flow characteristic sequence of each heat flow cluster, and the heat flow characteristic sequence is in a calcining area/>The method comprises the steps of obtaining mirror image clusters symmetrical to each heat flux cluster, arranging heat flux fully uniform coefficients of all pixels in each mirror image cluster in ascending order to serve as mirror image feature sequences of each mirror image cluster, and taking heat flux fully uniform coefficient average values of all pixels in each heat flux cluster as heat flux feature values of each heat flux cluster;
Calcination zone at time t Calcining sufficiency factor/>, of inner p-th thermal clusterThe expression of (2) is:
In the method, in the process of the invention, For the time t calcination zone/>Total number of pixels in inner p-th thermal cluster,/>、/>Calcination zone at time t/>, respectivelyThe heat flow of the q-th pixel in the inner p-th heat flow cluster is fully uniform in coefficient, and the heat flow characteristic value of the p-th heat flow cluster,/>For the time t calcination zone/>Heat flow characteristic value average value of all heat flow clusters in the reactor,/>For presetting the adjustment parameter larger than 0,/>Is a natural constant; by and calcine zone/>The calcining area/>, obtained by the same calculation method of calcining full factors of all the hot clusters in the reactorCalcining the full factors of each mirror image cluster;
Calcination zone at time t Heat transfer symmetry factor/>, of inner p-th heat clusterThe expression of (2) is:
In the method, in the process of the invention, 、/>Calcination zone at time t/>, respectivelyCalcining sufficiency factor of inner p-th thermal cluster, calcining sufficiency factor of mirror image cluster of p-th thermal cluster,/>For the time t calcination zone/>Total number of hot clusters in/(、/>Calcination zone at time t/>, respectivelyThe heat flow characteristic sequence of the inner p-th heat flow cluster, the mirror image characteristic sequence of the mirror image cluster of the p-th heat flow cluster,/>At dtw distance,/>Presetting an adjustment parameter larger than 0;
calcining the zone at each moment The normalized value of the heat transfer symmetry factor mean value of all the heat clusters in the furnace is used as the calcining sufficiency of the infrared thermal imaging image at each moment.
10. The method for preparing the special heat preservation material for the isostatic pressing graphite, which is disclosed in claim 1, is characterized in that the method for adjusting the calcining time length of the mixture in the calciner according to the calcining sufficiency of the infrared thermal imaging image at each moment comprises the following steps:
And calculating the calcining sufficiency of the infrared thermal imaging image at each moment, and if the calcining sufficiency is smaller than a preset calcining sufficiency threshold, prolonging the calcining time for 1min until the calcining sufficiency is greater than or equal to the preset calcining sufficiency threshold or the calcining time length reaches 1.5h.
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