A meta - p - cresol adsorbent based on porous materials and its preparation method

Abstract

The present invention relates to the technical field of chemical material preparation, and particularly to a meta - p - cresol adsorbent based on porous materials and a preparation method thereof. In the present invention, the raw material mixture is stirred, characteristic points of the stripe are marked according to the surface image of the raw material mixture, the contour of the characteristic stripe is determined to determine the sampling time window, the stripe characteristic points and stripe reference points are sampled and the samples are stained, local reference points are screened according to the comparison of the gray - scale values after staining, additional compensatory stirring is performed on the raw material mixture with local reference points during the stirring process, the stirring parameters of the compensatory stirring are determined according to the local reference points, and the stirred raw material mixture is subjected to crystallization control, pore - expanding modification and surface functionalization to obtain the target meta - p - cresol adsorbent. Furthermore, the stirring state of the mixture is monitored in a timely manner during the preparation process, the stirring method is adjusted adaptively according to different stirring states, and the structural uniformity of the meta - p - cresol adsorbent is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical material preparation, and particularly relates to a meta - p - cresol adsorbent based on porous material and a preparation method thereof. Background Art

[0002] Meta - p - cresol is an important organic chemical raw material, which is widely used in fields such as pesticides, pharmaceuticals, fragrances, dyes, etc. However, it has strong irritation and corrosiveness. If the wastewater containing meta - p - cresol is directly discharged without effective treatment, it will pose a threat to the environment and human health. The adsorption method can separate meta - p - cresol from wastewater through physical or chemical interactions between the adsorbent and meta - p - cresol. HZSM - 5 molecular sieve is a silicate material with a unique pore structure and acidity, having a large specific surface area and regular microporous structure, which can provide abundant adsorption sites. It can be transformed into an efficient meta - p - cresol adsorbent through hydrothermal synthesis - pore expansion modification - surface functionalization, which is more conducive to the diffusion and adsorption of meta - p - cresol molecules. However, during the hydrothermal synthesis process for preparing the meta - p - cresol adsorbent, the mixing of reactants such as silicon source, aluminum source, and template agent in the solution is not sufficient, resulting in differences in local concentration, affecting the structural uniformity and performance stability of the meta - p - cresol adsorbent. Therefore, it is an urgent technical problem to timely monitor the stirring state and adaptively adjust the process to improve the structural uniformity of the meta - p - cresol adsorbent.

[0003] For example, the Chinese patent application publication number: CN117861611A. This invention discloses a preparation method of a meta - p - cresol isomer separation and purification adsorbent. After the LSX molecular sieve with an Si / Al atomic ratio in the range of 1.0 - 1.1 is fully stirred and mixed with pillared bentonite and polyacrylamide and then formed into balls, it is exchanged with IA group and IIA group metal cations, and then processed through drying, dehydration activation, etc. to obtain the formed adsorbent. The formed adsorbent is filled into a counter - current simulated moving bed to realize continuous feeding of meta - p - cresol materials, desorbent, and continuous extraction of extract and raffinate materials, and finally obtain high - purity meta - cresol and p - cresol products.

[0004] The following problems also exist in the prior art:

[0005] The prior art does not consider that during the process of preparing the meta - p - cresol adsorbent using HZSM - 5 molecular sieve as the porous material, the insufficient mixing of reactants such as silicon source, aluminum source, and template agent will lead to inconsistent reaction processes in different parts of the mixture, thus affecting the pore structure. The prior art cannot timely monitor the stirring state of the mixture during the preparation process and cannot adaptively adjust the stirring method according to different stirring states, affecting the structural uniformity of the preparation of the meta - p - cresol adsorbent. Summary of the Invention

[0006] To this end, the present invention provides a meta - p - cresol adsorbent based on porous materials and a preparation method thereof, so as to overcome the problem in the prior art that the stirring state of the mixture cannot be monitored in time during the preparation process, and the stirring method cannot be adjusted adaptively according to different stirring states, which affects the structural uniformity of the preparation of the meta - p - cresol adsorbent.

[0007] To achieve the above object, the present invention provides a preparation method of a meta - p - cresol adsorbent based on porous materials, including:

[0008] Mix the raw materials required for preparation into a raw material mixture according to preset components and stir.

[0009] Obtain the surface images of the raw material mixture at several moments within a preset acquisition period, mark the stripe feature points according to the stripe contour in the surface image and determine the characteristic stripe contour, and obtain the change in the number of stripe feature points at each moment in time sequence to determine the sampling time window of the raw material mixture.

[0010] Sample the stripe feature points and stripe reference points on the characteristic stripe contour within the sampling time window.

[0011] Dye the characteristic samples collected at the stripe feature points and the reference samples collected at the stripe reference points, and screen the local reference points according to the comparison of the gray - scale values after dyeing.

[0012] Add compensated stirring to the raw material mixture with local reference points during the stirring process, and determine the stirring parameters for compensated stirring of the characteristic stripe contour according to the number of local reference points on the characteristic stripe contour, including:

[0013] Determine the stirring center point of the compensated stirring according to the comparison of the gray - scale values of the characteristic samples at several local reference points, and determine the stirring radius of the compensated stirring according to the interval distance between the stirring center point and each local reference point.

[0014] Or, use the local reference point as the stirring center point of the compensated stirring, and determine the stirring radius of the compensated stirring according to the comparison of the gray - scale values at the local reference point.

[0015] Perform crystallization control, pore - expansion modification, and surface functionalization on the raw material mixture after completion of stirring to obtain the target meta - p - cresol adsorbent.

[0016] Further, the process of marking the stripe feature points and determining the characteristic stripe contour includes:

[0017] Identify the stripe discontinuity points in the surface image.

[0018] If the tangent directions of the stripe profile endpoints on both sides of the stripe discontinuity point are the same, the stripe profiles on both sides of the stripe discontinuity point are combined and determined as the characteristic stripe profile, and the stripe discontinuity point is marked as the stripe feature point.

[0019] Further, the process of determining the sampling time window of the raw material mixture includes

[0020] Set several acquisition times within a preset acquisition period, calculate the difference between the number of stripe feature points in the surface image at the subsequent acquisition time and the number of stripe feature points in the surface image at the previous acquisition time respectively, and combine the differences into a sequence in time series;

[0021] If the sequence is an increasing sequence, the last acquisition time within the acquisition period is determined as the sampling time window of the raw material mixture;

[0022] If the sequence is not an increasing sequence, the raw material mixture is not sampled.

[0023] Further, only one stripe reference point is marked on each characteristic stripe profile, and the stripe reference point is a point on the characteristic stripe profile other than the stripe feature point.

[0024] Further, the process of screening local reference points includes

[0025] Obtain the first gray value after staining the characteristic sample collected at the stripe feature point, and the second gray value after staining the reference sample collected at the stripe reference point of the characteristic stripe profile where the stripe feature point is located;

[0026] Calculate the absolute value of the difference between the first gray value and the second gray value, and determine the absolute value of the difference as the content characterization value of the stripe feature point;

[0027] If the content characterization value of the stripe feature point meets the reference point determination condition, the stripe feature point is screened as a local reference point;

[0028] Among them, the reference point determination condition is that the content characterization value exceeds a preset content reference value.

[0029] Further, the process of determining the stirring parameters for compensating stirring of the characteristic stripe profile includes

[0030] If the number of local reference points on the characteristic stripe profile exceeds 1, determine the stirring center point of the compensating stirring according to the comparison of the gray values of the characteristic samples at several local reference points, and determine the stirring radius of the compensating stirring according to the interval distance between the stirring center point and each local reference point;

[0031] If the number of local reference points on the contour of the characteristic stripe is 1, the local reference point is used as the stirring center point of the compensating stirring, and the stirring radius of the compensating stirring is determined according to the comparison of the gray scale values at the local reference point;

[0032] If the number of local reference points on the contour of the characteristic stripe is 0, no stirring center point and stirring radius are set for the contour of the characteristic stripe.

[0033] Further, according to the determination result that the number of local reference points on the contour of the characteristic stripe exceeds 1, the content characterization values of the local reference points on the contour of the characteristic stripe are obtained, and the local reference point corresponding to the maximum content characterization value is determined as the stirring center point.

[0034] Further, according to the determination result that the number of local reference points on the contour of the characteristic stripe exceeds 1, the interval distances between the stirring center point and the other local reference points are obtained, and the maximum interval distance is determined as the stirring radius.

[0035] Further, according to the determination result that the number of local reference points on the contour of the characteristic stripe is 1, the stirring radius is positively correlated with the content characterization value of the local reference point.

[0036] The present invention also provides an m - cresol adsorbent based on porous materials, comprising:

[0037] Silica and aluminum oxide with a molar ratio of 100:1, 70% - 90%, ferric chloride solution 5% - 20%, and mesoporous alumina 10% - 25%.

[0038] Compared with the prior art, the beneficial effects of the present invention are as follows: by mixing the raw materials required for preparation into a raw material mixture according to preset components and stirring, surface images of the raw material mixture at several moments within a preset acquisition period are obtained, stripe feature points are marked and the characteristic stripe contour is determined according to the stripe contour in the surface image, the change situation of the number of stripe feature points at each moment is obtained in chronological order to determine the sampling moment window of the raw material mixture, sampling is performed on the stripe feature points and stripe reference points on the characteristic stripe contour at the sampling moment window, the characteristic samples collected at the stripe feature points and the reference samples collected at the stripe reference points are dyed, local reference points are screened according to the comparison of the gray scale values after dyeing, compensating stirring is added during the stirring process of the raw material mixture with local reference points, the stirring parameters for compensating stirring of the characteristic stripe contour are determined according to the number of local reference points on the characteristic stripe contour, and the raw material mixture after completion of stirring is subjected to crystallization control, pore expansion modification, and surface functionalization to prepare the target m - cresol adsorbent. Furthermore, the stirring state of the mixture is monitored in a timely manner during the preparation process, the stirring method is adjusted adaptively according to different stirring states, and the structural uniformity of the preparation of the m - cresol adsorbent is improved.

[0039] In particular, according to the present invention, stripe feature points are marked based on the stripe contour in the surface image and the characteristic stripe contour is determined. It can be understood that the stripes in the surface image of the raw material mixture are the external manifestations of its internal mixing situation. By marking the stripe feature points and determining the characteristic stripe contour, information such as the non-uniformity of the raw material mixture and the difference in the reaction process can be intuitively presented, and the mixing uniformity of the raw material mixture can be quantitatively evaluated. Through the analysis of the surface image, problems existing in the raw material mixture can be timely detected. By marking the stripe feature points and determining the characteristic stripe contour in the surface image, furthermore, specific data support is provided for quality control during the preparation process, the stirring state of the mixture is timely monitored during the preparation process, and the structural uniformity of the preparation of m-cresol adsorbent is improved.

[0040] In particular, according to the present invention, the change in the number of stripe feature points at each moment is obtained in chronological order to determine the sampling time window of the raw material mixture. It can be understood that during the stirring process of the raw material mixture, its internal mixing state changes continuously with time, and the number of stripe feature points can reflect the uniformity of this mixing and the reaction process. By recording the change in this number in chronological order, the trend of the mixing state of the mixture can be accurately obtained. Sampling at the appropriate time point can make the sample more representative, provide a reliable basis for subsequent analysis and preparation, reduce invalid sampling, avoid sampling costs and time consumption. By obtaining the change in the number of stripe feature points at each moment in chronological order to determine the sampling time window of the raw material mixture, furthermore, the stirring state of the mixture is timely monitored during the preparation process, the sampling efficiency is improved, the production cost is reduced, and the preparation efficiency of m-cresol adsorbent is improved.

[0041] In particular, according to the present invention, the stripe feature points and stripe reference points on the characteristic stripe contour are sampled within the sampling time window. It can be understood that the characteristic samples at the stripe feature points and the reference samples at the stripe reference points of the characteristic stripe contour where the stripe feature points are located both belong to the raw material mixture on the same stripe contour. By comparing the two, the component distribution state of the mixture can be more comprehensively understood, and the representativeness of the comparison data can be improved. By sampling the stripe feature points and stripe reference points on the characteristic stripe contour within the sampling time window, furthermore, the stirring state of the mixture is timely monitored during the preparation process, and the structural uniformity of the preparation of m-cresol adsorbent is improved.

[0042] In particular, the present invention screens local reference points based on the comparison of gray values after staining. It can be understood that the stripe feature points recognized from the surface image of the raw material mixture may be misjudged due to insufficient image recognition accuracy. After staining the sample, its gray value will vary depending on the component content in the sample. By comparing the gray values of the stripe feature points and the stripe reference points, the actual stripe discontinuity points on the surface of the mixture can be screened out to avoid misjudgment. Furthermore, the stirring state of the mixture can be monitored in a timely manner during the preparation process, improving the structural uniformity of the preparation of the m - cresol adsorbent.

[0043] In particular, the present invention adds compensatory stirring to the raw material mixture with local reference points during the stirring process, and determines the stirring parameters for compensatory stirring of the characteristic stripe contour according to the number of local reference points on the characteristic stripe contour. It can be understood that compensatory stirring can enable the raw material mixture at the local reference points and the surrounding area to perform more sufficient mass exchange. Under the action of compensatory stirring, the materials with different components around the discontinuity points are stirred up, accelerating the molecular diffusion and convection processes, enabling the component at the local reference point with component differences to more quickly tend to be consistent with the components of the overall material, thereby improving the uniformity of the entire raw material mixture. Determining the compensatory stirring method according to the number of local reference points can achieve targeted stirring of the characteristic stripe contour and reach a high degree of mixing uniformity in a short time. The present invention adds compensatory stirring to the raw material mixture with local reference points during the stirring process, determines the stirring parameters for compensatory stirring of the characteristic stripe contour according to the number of local reference points on the characteristic stripe contour, and further, monitors the stirring state of the mixture in a timely manner during the preparation process, adaptively adjusts the stirring method according to different stirring states, and improves the structural uniformity of the preparation of the m - cresol adsorbent. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 It is the logic flowchart of the preparation method of the m - cresol adsorbent based on porous materials according to the embodiment of the present invention;

[0045] Figure 2 It is the logic flowchart of determining the sampling time window of the raw material mixture according to the embodiment of the present invention;

[0046] Figure 3 It is the logic flowchart of screening local reference points according to the embodiment of the present invention;

[0047] Figure 4 It is the logic flowchart of determining the stirring parameters for compensatory stirring of the characteristic stripe contour according to the embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0048] To make the objectives and advantages of the present invention more clear and understandable, the present invention will be further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0049] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are only used to explain the technical principles of the present invention and do not limit the protection scope of the present invention.

[0050] It should be noted that in the description of the present invention, the terms indicating the direction or positional relationship such as "upper", "lower", "inner", "outer", etc. are based on the direction or positional relationship shown in the drawings. This is only for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation to the present invention.

[0051] Please refer to Figure 1 As shown, it is a logic flowchart of the preparation method of the m - cresol and p - cresol adsorbent based on porous materials according to the embodiment of the present invention. The preparation method of the m - cresol and p - cresol adsorbent based on porous materials of the present invention includes:

[0052] Step S100, mixing the raw materials required for preparation into a raw material mixture according to a preset composition and stirring.

[0053] Specifically, the preset composition may include 75% of silica and alumina with a molar ratio of 100:1, 10% ferric chloride solution, 10% alumina, and 5% binder. The binder may be silica sol, which will not be elaborated here.

[0054] Step S200, obtaining the surface images of the raw material mixture at several moments within a preset acquisition period, marking the stripe feature points according to the stripe contours in the surface images and determining the characteristic stripe contours, and obtaining the change of the number of stripe feature points at each moment in time sequence to determine the sampling moment window of the raw material mixture.

[0055] Specifically, the preset acquisition period can be set by those skilled in the art according to the precision requirements for the preparation of the m - cresol and p - cresol adsorbent. The higher the precision requirements, the longer the preset acquisition period. Preferably, the duration of the preset acquisition period can be 20 min.

[0056] Step S300, sampling the stripe feature points and stripe reference points on the characteristic stripe contours within the sampling moment window.

[0057] Specifically, the present invention samples the stripe feature points and stripe reference points on the feature stripe profile at the sampling time window. It can be understood that the feature samples at the stripe feature points and the reference samples at the stripe reference points of the feature stripe profile where the stripe feature points are located both belong to the raw material mixture on the same stripe profile. By comparing the two, the composition distribution state of the mixture can be more comprehensively understood, and the representativeness of the comparison data can be improved. The present invention samples the stripe feature points and stripe reference points on the feature stripe profile at the sampling time window. Furthermore, the stirring state of the mixture is monitored in a timely manner during the preparation process, and the structural uniformity of the preparation of m - cresol adsorbent is improved.

[0058] Specifically, the sampling amount for sampling the stripe feature points and stripe reference points can be the product of the total amount of the raw material mixture and the sampling amount value factor. The sampling amount value factor can be set by those skilled in the art according to the precision requirements for the preparation of m - cresol adsorbent. The higher the precision requirements, the larger the sampling amount value factor. The value range of the sampling amount value factor can be [0.02, 0.04]. Preferably, the sampling amount value factor can be 0.02.

[0059] Step S400: Stain the feature samples collected at the stripe feature points and the reference samples collected at the stripe reference points, and screen local reference points according to the comparison of the gray - scale values after staining;

[0060] Specifically, the same content of a staining agent is added to the collected feature samples and reference samples. The staining agent can be silver nitrate. The addition amount of the staining agent can be set by those skilled in the art according to the sampling amount. When the sampling amount is 20 g, the value range of the addition amount can be [0.05, 0.5], and the interval unit is g. If the addition amount is too small, the ideal staining effect cannot be achieved, making it difficult to screen local reference points through the comparison of gray - scale values. If the addition amount is too large, over - staining will occur, which not only causes waste of reagents but also affects the subsequent observation and analysis of the samples. Preferably, the addition amount can be 0.2 g.

[0061] Step S500: Increase the compensatory stirring during the stirring process of the raw material mixture with local reference points, and determine the stirring parameters for the compensatory stirring of the feature stripe profile according to the number of local reference points on the feature stripe profile, including,

[0062] Determine the stirring center point of the compensatory stirring according to the comparison of the gray - scale values of the feature samples at several local reference points, and determine the stirring radius of the compensatory stirring according to the interval distance between the stirring center point and each local reference point;

[0063] Or, use the local reference point as the stirring center point of the compensatory stirring, and determine the stirring radius of the compensatory stirring according to the comparison of the gray - scale values at the local reference point;

[0064] Specifically, the telescopic movement of the blades can be driven by a hydraulic or electric push rod through multi-layer nested blades to continuously adjust the stirring radius, and the offset of the eccentric shaft can be controlled by a rack and pinion or a linear motor to adjust the stirring center, which will not be elaborated here.

[0065] Specifically, the present invention adds compensatory stirring to the raw material mixture with local reference points during the stirring process, and determines the stirring parameters for compensatory stirring of the characteristic stripe profile according to the number of local reference points on the characteristic stripe profile. It can be understood that the compensatory stirring can enable the raw material mixture at the local reference points and the surrounding areas to carry out material exchange more fully. Under the action of the compensatory stirring, the materials with different components around the discontinuous points are stirred up, accelerating the molecular diffusion and convection processes, so that at the local reference points with component differences, they can more quickly tend to be consistent with the components of the whole material, thereby improving the uniformity of the entire raw material mixture. Determining the compensatory stirring method according to the number of local reference points can achieve targeted stirring of the characteristic stripe profile and reach a high mixing uniformity in a short time. The present invention adds compensatory stirring to the raw material mixture with local reference points during the stirring process, determines the stirring parameters for compensatory stirring of the characteristic stripe profile according to the number of local reference points on the characteristic stripe profile, and further, realizes the timely monitoring of the stirring state of the mixture during the preparation process, adaptively adjusts the stirring method according to different stirring states, and improves the structural uniformity of the preparation of the m-cresol adsorbent.

[0066] Step S600: Subject the stirred raw material mixture to crystallization control, pore expansion modification, and surface functionalization to obtain the target m-cresol adsorbent.

[0067] Specifically, crystallization control is carried out at a reaction temperature of 150°C to 180°C and a reaction pressure value of 0.8 MPa to 1.5 MPa in a reaction kettle for 24 h to 48 h to directionally construct a molecular sieve framework to form a stable microporous structure. Preferably, the reaction temperature in the crystallization control can be 160°C, the reaction pressure value can be 1.2 MPa, and the reaction duration can be 30 h. The acid etching method is used to selectively dissolve the non-framework aluminum of the molecular sieve with dilute nitric acid at a concentration of 0.1 mol / L to 0.5 mol / L to generate secondary pores for pore expansion modification to improve the mass transfer efficiency and relieve micropore blockage. Preferably, the dilute nitric acid can be 0.25 mol / L. Surface functionalization is carried out by impregnating a copper sulfate solution at a concentration of 0.5 mol / L to 1.0 mol / L and performing static ion exchange at 60°C for 6 h to 12 h to enhance the adsorption selectivity and improve the adsorption stability. Preferably, the copper sulfate solution can be 0.85 mol / L, and the static ion exchange duration can be 8 h, which will not be elaborated here.

[0068] Specifically, the process of marking stripe feature points and determining the contour of the feature stripe includes

[0069] identifying the discontinuity points of the stripes in the surface image;

[0070] If the tangent directions of the stripe contour endpoints on both sides of the stripe discontinuity point are the same, then the stripe contours on both sides of the stripe discontinuity point are merged and determined as the feature stripe contour, and the stripe discontinuity point is marked as the stripe feature point.

[0071] Specifically, the surface image of the raw material mixture can be obtained by an industrial camera, and the edge algorithm is used to identify the discontinuity points of the stripes, the stripe contours, and the tangent directions of the stripe contour endpoints in the surface image. The microprocessor is used to mark the stripe feature points and determine the feature stripe contour. This is the prior art and will not be elaborated here.

[0072] Specifically, the present invention marks the stripe feature points and determines the feature stripe contour according to the stripe contour in the surface image. It can be understood that the stripes in the surface image of the raw material mixture are the external manifestations of its internal mixing conditions. By marking the stripe feature points and determining the feature stripe contour, information such as the non-uniformity of the raw material mixing and the differences in the reaction process can be intuitively presented, and the mixing uniformity of the raw material mixture can be quantitatively evaluated. Through the analysis of the surface image, the problems existing in the raw material mixture can be found in time. The present invention marks the stripe feature points and determines the feature stripe contour through the stripe contour in the surface image, and further, provides specific data support for quality control in the preparation process, monitors the stirring state of the mixture in time during the preparation process, and improves the structural uniformity of the preparation of the m-cresol adsorbent.

[0073] Specifically, reflecting the stirring and mixing state, when the raw material mixture is stirred, if the stirring is uniform, the fluid should present a relatively uniform flow state and the raw material distribution is also relatively uniform. When the stirring is non-uniform, uneven distributions of velocity gradient and shear stress will be generated. In the region with a large shear stress, the fluid is stretched and deformed, resulting in local concentration changes of the raw materials. This non-uniformity will cause the reaction process in some regions to be faster than that in other regions, forming stripe-shaped gels. The stripe feature points are the discontinuity points on the stripe-shaped gels with the same orientation. The formation of the discontinuity points on the stripe-shaped gels is due to the non-uniform distribution of the mixture. The raw material composition at the discontinuity points is less, and the reaction process is slower than that at the adjacent gels. Therefore, discontinuity points are formed on the stripe-shaped gels. By marking the stripe feature points and determining the feature stripe contour through the stripe contour in the surface image, and further, provides specific data support for quality control in the preparation process, monitors the stirring state of the mixture in time during the preparation process, and improves the structural uniformity of the preparation of the m-cresol adsorbent.

[0074] Specifically, please refer to Figure 2As shown, it is a logic flowchart for determining the sampling time window of the raw material mixture in an embodiment of the present invention. The process of determining the sampling time window of the raw material mixture includes:

[0075] Set several acquisition times within a preset acquisition period, calculate the difference between the number of stripe feature points in the surface image at the subsequent acquisition time and the number of stripe feature points in the surface image at the previous acquisition time respectively, and combine the differences into a sequence in time order;

[0076] If the sequence is an increasing sequence, determine the last acquisition time within the acquisition period as the sampling time window of the raw material mixture;

[0077] If the sequence is not an increasing sequence, do not sample the raw material mixture.

[0078] In practice, the interval duration of the acquisition times set within the preset acquisition period can be 2 minutes, and 10 acquisition times are set. Exemplarily, a specific method for determining the sampling time window of the raw material mixture is given here. If the numbers of stripe feature points in the surface images at 10 acquisition times within the acquisition period are obtained as: 2, 3, 5, 9, 14, 21, 30, 40, 52, 65, calculate the differences between the number of stripe feature points in the surface image at the subsequent acquisition time and the number of stripe feature points in the surface image at the previous acquisition time respectively as: 1, 2, 4, 5, 7, 9, 10, 12, 13, and combine the differences into a sequence {1, 2, 4, 5, 7, 9, 10, 12, 13}, which is an increasing sequence. Therefore, the tenth acquisition time is determined as the sampling time window of the raw material mixture.

[0079] Specifically, the present invention obtains the change situation of the number of stripe feature points at each time in time order to determine the sampling time window of the raw material mixture. It can be understood that during the stirring process of the raw material mixture, its internal mixing state changes continuously with time, and the number of stripe feature points can reflect the uniformity of this mixing and the reaction process. By recording the change of this number in time order, the trend of the mixing state of the mixture can be accurately grasped. Sampling at the appropriate time point can make the sample more representative, provide a reliable basis for subsequent analysis and preparation, reduce ineffective sampling, avoid sampling costs and time consumption. The present invention obtains the change situation of the number of stripe feature points at each time in time order to determine the sampling time window of the raw material mixture. Furthermore, it realizes the timely monitoring of the stirring state of the mixture during the preparation process, improves the sampling efficiency, reduces the production cost, and improves the efficiency of preparing p-cresol adsorbent.

[0080] Specifically, the present invention obtains the change in the number of stripe feature points at each moment in time sequence to determine the sampling time window of the raw material mixture. It can be understood that when stirring the raw material mixture, the stirring equipment causes the mixture to flow and tumble through mechanical action. According to fluid mechanics, the shear force and turbulent kinetic energy generated by stirring will promote the mutual mixing of the materials, making the originally unevenly distributed raw materials gradually tend to be uniform. The continuous action of stirring enables the raw materials to come into full contact and react at the microscale, reducing the local concentration difference, and the number of stripe feature points will also decrease accordingly. During the preset acquisition period, when the difference between the number of stripe feature points in the surface image at the latter acquisition moment and the number of stripe feature points in the surface image at the previous acquisition moment is on an increasing trend, it indicates that the number of stripe feature points does not decrease with the increase of the stirring time, and the uniformity of the raw material mixture does not improve. The last acquisition moment within the preset acquisition period reflects the moment when the uniformity of the raw material mixture is the worst. Determining it as the sampling time window can improve the data representativeness of the sampling. The present invention obtains the change in the number of stripe feature points at each moment in time sequence to determine the sampling time window of the raw material mixture, thereby improving the data representativeness of the sampling, reducing the production cost, and improving the efficiency of preparing the m-cresol adsorbent.

[0081] Specifically, only one stripe reference point is marked on each characteristic stripe contour, and the stripe reference point is a point on the characteristic stripe contour other than the stripe feature points.

[0082] Specifically, please refer to Figure 3 as shown, which is the logic flow chart for screening local reference points in the embodiment of the present invention. The process of screening local reference points includes

[0083] obtaining the first gray value after staining the characteristic sample collected at the stripe feature point, and the second gray value after staining the reference sample collected at the stripe reference point of the characteristic stripe contour where the stripe feature point is located;

[0084] calculating the absolute value of the difference between the first gray value and the second gray value, and determining the absolute value of the difference as the content characterization value of the stripe feature point;

[0085] Specifically, the determination of the gray value can be achieved by using an industrial camera to obtain the stained sample image, and using an image processor to preprocess the obtained sample image. The preprocessing includes grayscale conversion, filtering and denoising, and contrast enhancement. The gray value in the preprocessed sample image is extracted using image analysis software, which will not be elaborated here.

[0086] Specifically, the gray value range of the first gray value of the feature sample collected at the stripe feature point after being stained with silver nitrate as a stain is [100, 200], and the gray value range of the second gray value of the reference sample collected at the stripe reference point of the feature stripe contour where the stripe feature point is located after being stained with silver nitrate as a stain is [100, 150].

[0087] If the content characterization value of the stripe feature point meets the benchmark point determination condition, then the stripe feature point is screened as a local benchmark point;

[0088] If the content characterization value of the stripe feature point does not meet the benchmark point determination condition, then the stripe feature point is not screened;

[0089] Among them, the benchmark point determination condition is that the content characterization value exceeds a preset content reference value.

[0090] Specifically, the preset content reference value can be the product of the second gray value and the content reference value factor. The content reference value factor can be set by those skilled in the art according to the precision requirements for the preparation of m - cresol adsorbent. The higher the precision requirement, the smaller the content reference value factor. The value range of the content reference value factor can be [0.2, 0.4]. Preferably, the content reference value factor can be 0.3.

[0091] Exemplarily, a specific method for determining the content characterization value of the stripe feature point is given here. The first gray value of the feature sample collected at the stripe feature point after staining is 180, and the second gray value of the reference sample collected at the stripe reference point of the feature stripe contour where the stripe feature point is located after staining is 120. The absolute value of the difference between the first gray value and the second gray value is 60. Therefore, the content characterization value is 60.

[0092] Specifically, the present invention screens local benchmark points according to the comparison of the gray values after staining. It can be understood that the stripe feature points recognized through the surface image of the raw material mixture may be misjudged due to insufficient image recognition accuracy. After staining the sample, its gray value will vary according to the different component contents in the sample. By comparing the gray values of the stripe feature points and the stripe reference points, the actual stripe discontinuity points on the surface of the mixture can be screened out to avoid misjudgment. Furthermore, the stirring state of the mixture can be monitored in a timely manner during the preparation process, and the structural uniformity of the preparation of m - cresol adsorbent is improved.

[0093] Specifically, there are incompletely reacted intermediates at the stripe discontinuities, which contain more active sites, acidic or basic groups, and have a stronger binding ability to metal ions. This will cause an increase in the adsorption amount of metal ions at the discontinuities. The adsorption of a relatively large amount of metal ions will lead to an enhanced absorption of light at specific wavelengths and a relatively weakened reflected light intensity, resulting in a larger gray value. In the reference sample obtained at the stripe reference points, the structure and composition of the aluminosilicate precursor are relatively stable, and the functional groups and charge distribution on its surface are also relatively uniform. When a metal ion dye is added, the metal ions will bind to specific groups on the surface of the aluminosilicate through ion exchange, coordination, etc. Due to the uniformity of the structure, the adsorption amount and distribution of metal ions at the stripes are relatively uniform, making the absorption and scattering of light at the stripes relatively stable and at a low level. Compared with the stripe discontinuities, it will not cause a large amount of light absorption or scattering due to factors such as structural defects and uneven metal ion distribution. Therefore, the reflected light intensity is relatively high, and it shows a smaller gray value in the imaging system. The present invention screens the actual stripe discontinuities as local reference points based on the comparison of the gray values after staining. Furthermore, it realizes the timely monitoring of the stirring state of the mixture during the preparation process and improves the structural uniformity of the preparation of the m-cresol adsorbent.

[0094] Specifically, please refer to Figure 4 As shown, it is a logic flowchart for determining the stirring parameters for compensating stirring of the characteristic stripe profile in an embodiment of the present invention. The process of determining the stirring parameters for compensating stirring of the characteristic stripe profile includes

[0095] If the number of local reference points on the characteristic stripe profile exceeds 1, the stirring center point of the compensating stirring is determined according to the comparison of the gray values of the characteristic samples at several local reference points, and the stirring radius of the compensating stirring is determined according to the interval distance between the stirring center point and each local reference point;

[0096] If the number of local reference points on the characteristic stripe profile is 1, the local reference point is used as the stirring center point of the compensating stirring, and the stirring radius of the compensating stirring is determined according to the comparison of the gray values at the local reference point;

[0097] If the number of local reference points on the characteristic stripe profile is 0, no stirring center point and stirring radius are set for the characteristic stripe profile.

[0098] Specifically, under the condition that the number of local reference points on the characteristic stripe contour of the present invention is 0, no stirring center point and stirring radius are set for the characteristic stripe contour. It can be understood that when the number of local reference points on the characteristic stripe contour is 0, within the region corresponding to the characteristic stripe contour, the composition of the raw material mixture is relatively uniform, and there are no obvious non-uniform points that require special treatment. Therefore, there is no need to set a stirring center point and a stirring radius for targeted compensatory stirring. In addition, there will be other characteristic stripes containing local reference points that require compensatory stirring, and the compensatory stirring performed will also make the composition of the raw material mixture at the characteristic stripe contour without local reference points more uniform. Furthermore, the stirring state of the mixture is monitored in a timely manner during the preparation process, and the stirring method is adaptively adjusted according to different stirring states, improving the structural uniformity of the preparation of m - cresol adsorbent.

[0099] Specifically, according to the determination result that the number of local reference points on the characteristic stripe contour exceeds 1, the content characterization values of each local reference point on the characteristic stripe contour are obtained, and the local reference point corresponding to the maximum content characterization value is determined as the stirring center point.

[0100] Specifically, according to the determination result that the number of local reference points on the characteristic stripe contour exceeds 1, the interval distances between the stirring center point and the remaining local reference points are obtained, and the maximum interval distance is determined as the stirring radius.

[0101] Specifically, under the condition that the number of local reference points on the characteristic stripe contour of the present invention exceeds 1, the stirring center point for compensatory stirring is determined according to the comparison of the gray - scale values of the characteristic samples at the local reference points, and the stirring radius for compensatory stirring is determined according to the interval distances between the stirring center point and each local reference point. It can be understood that the comparison of the gray - scale values of the characteristic samples at the local reference points can reflect the differences in the composition of the raw material mixture. The larger the content reference value, the more significant the composition difference between this local reference point and the adjacent region. Determining the local reference point with the largest difference as the stirring center point can perform key stirring on the region with the largest composition difference, helping to quickly improve the uniformity of the raw material mixture and reduce the overall composition deviation. Determining the stirring radius according to the interval distances between the stirring center point and each local reference point can ensure that the stirring effect effectively covers all non - uniform regions that need to be improved. Based on the distances between these points and the stirring center point, it can be ensured that during the stirring process, the regions where other local reference points are located can also be affected by the stirring effect, thereby realizing the uniform mixing of the raw material mixture in the entire characteristic stripe contour region. Furthermore, the stirring state of the mixture is monitored in a timely manner during the preparation process, and the stirring method is adaptively adjusted according to different stirring states, improving the structural uniformity of the preparation of m - cresol adsorbent.

[0102] Specifically, according to the determination result that the number of local reference points on the characteristic stripe profile is 1, the stirring radius is positively correlated with the content characterization value of the local reference points.

[0103] Exemplarily, here is a specific method for determining the stirring radius under the condition that the number of local reference points on the characteristic stripe profile is 1. The stirring radius is the product of the content characterization value and the stirring radius value factor. The value range of the stirring radius value factor can be [0.2, 0.4]. If the value of the stirring radius value factor is too large, it will lead to an overly large stirring range, causing unnecessary energy consumption. If the value is too small, it will not be able to fully cover the area that needs to be stirred. Preferably, the stirring radius value factor can be 0.3. The content characterization value of the local reference point is 80, and the stirring radius is 24. The unit of the stirring radius is cm.

[0104] Specifically, under the condition that the number of local reference points on the characteristic stripe profile of the present invention is 1, using the local reference point as the stirring center point for compensated stirring, the stirring radius of the compensated stirring is determined according to the comparison of the gray values at the local reference point. It can be understood that when the number of local reference points is 1, this point is a significant identifier of the non-uniformity in the raw material mixture, representing the position with the largest difference across the entire characteristic stripe profile. Using it as the stirring center point can directly stir this key area, specifically addressing the local non-uniformity problem in the raw material mixing. The content characterization value can reflect the degree of compositional difference between this local reference point and other areas of the characteristic stripe profile. The larger the content characterization value, the more obvious the difference, and a larger stirring radius is required to fully mix it with the surrounding raw material mixture to achieve uniformization. Furthermore, it realizes the timely monitoring of the stirring state of the mixture during the preparation process, adaptively adjusting the stirring method according to different stirring states, and improving the structural uniformity of the preparation of the m - cresol adsorbent.

[0105] The m - cresol adsorbent based on porous materials of the present invention comprises:

[0106] Silica and alumina with a molar ratio of 100:1, 70% - 85%, iron chloride solution 5% - 15%, mesoporous alumina 10% - 20%.

[0107] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will all fall within the protection scope of the present invention.

[0108] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention; for those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A preparation method of a meta - p - cresol adsorbent based on porous materials, characterized in that, Including: Mix the raw materials required for preparation into a raw material mixture according to preset components and stir; Obtain the surface images of the raw material mixture at several moments within a preset acquisition period, mark the stripe feature points according to the stripe contours in the surface images and determine the characteristic stripe contours, and obtain the change in the number of stripe feature points at each moment in chronological order to determine the sampling moment window of the raw material mixture; Sample the stripe feature points and stripe reference points on the characteristic stripe contour within the sampling moment window; Dye the characteristic samples collected at the stripe feature points and the reference samples collected at the stripe reference points, and screen the local reference points according to the comparison of the gray values after dyeing; Add compensatory stirring to the raw material mixture with local reference points during the stirring process, and determine the stirring parameters for compensatory stirring of the characteristic stripe contour according to the number of local reference points on the characteristic stripe contour, including If the number of local reference points on the characteristic stripe contour exceeds 1, determine the stirring center point of the compensatory stirring according to the comparison of the gray values of the characteristic samples at several local reference points, and determine the stirring radius of the compensatory stirring according to the interval distance between the stirring center point and each local reference point; If the number of local reference points on the characteristic stripe contour is 1, use the local reference point as the stirring center point of the compensatory stirring, and determine the stirring radius of the compensatory stirring according to the comparison of the gray values at the local reference point; If the number of local reference points on the characteristic stripe contour is 0, no stirring center point and stirring radius are set for the characteristic stripe contour; Perform crystallization control, pore expansion modification, and surface functionalization on the stirred raw material mixture to prepare the target m - cresol adsorbent; Among them, the process of determining the sampling moment window of the raw material mixture is to set several acquisition moments within a preset acquisition period, calculate the difference between the number of stripe feature points in the surface image at the latter acquisition moment and the number of stripe feature points in the surface image at the previous acquisition moment respectively, and combine the differences into a sequence in chronological order; If the sequence is an increasing sequence, determine the last acquisition moment within the acquisition period as the sampling moment window of the raw material mixture; If the sequence is not an increasing sequence, no sampling is performed on the raw material mixture; The process of marking the stripe feature points and determining the characteristic stripe contour includes identifying the stripe discontinuity points in the surface image; If the tangent directions of the stripe contour endpoints on both sides of the stripe discontinuity point are the same, merge the stripe contours on both sides of the stripe discontinuity point to determine the characteristic stripe contour, and mark the stripe discontinuity point as the stripe feature point; The process of screening the local reference points according to the comparison of the gray values after dyeing includes obtaining the first gray value after dyeing of the characteristic samples collected at the stripe feature points and the second gray value after dyeing of the reference samples collected at the stripe reference points of the characteristic stripe contour where the stripe feature points are located; Calculate the absolute value of the difference between the first gray value and the second gray value, and determine the content characterization value of the stripe feature point with the absolute value of the difference; If the content characterization value of the stripe feature points meets the benchmark point determination condition, the stripe feature points are screened as local benchmark points, and the benchmark point determination condition is that the content characterization value exceeds a preset content reference value.

2. The preparation method of the m - cresol and p - cresol adsorbent based on porous materials according to claim 1, wherein, Only one stripe reference point is marked on each characteristic stripe contour, and the stripe reference point is a point on the characteristic stripe contour other than the stripe feature points.

3. The preparation method of the m - cresol and p - cresol adsorbent based on porous materials according to claim 2, wherein, According to the determination result that the number of local benchmark points on the characteristic stripe contour exceeds 1, obtain the content characterization values of each local benchmark point on the characteristic stripe contour, and determine the local benchmark point corresponding to the maximum content characterization value as the stirring center point.

4. The preparation method of the m / p-cresol adsorbent based on porous materials according to claim 3, characterized in that, According to the determination result that the number of local benchmark points on the characteristic stripe contour exceeds 1, obtain the spacing distance between the stirring center point and the remaining local benchmark points, and determine the maximum spacing distance as the stirring radius.

5. The preparation method of the m - cresol and p - cresol adsorbent based on porous materials according to claim 4, characterized in that According to the determination result that the number of local benchmark points on the characteristic stripe contour is 1, the stirring radius is positively correlated with the content characterization value of the local benchmark point.

6. A meta - p - cresol adsorbent based on porous materials, which is prepared by using the preparation method of the meta - p - cresol adsorbent based on porous materials according to any one of claims 1 - 5 above, characterized in that, The raw materials include: Silica and alumina with a molar ratio of 100:1, 70% - 90%, ferric chloride solution 5% - 20%, mesoporous alumina 10% - 25%.

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