Porous material-based m-cresol and p-cresol adsorbent and preparation method thereof

Abstract

The invention relates to the technical field of chemical material preparation, in particular to a m-cresol and p-cresol adsorbent based on a porous material and a preparation method thereof.The preparation method comprises the steps that a raw material mixture is stirred, stripe feature points are marked according to a surface image of the raw material mixture, and feature stripe contours are determined so as to determine a sampling time window; sampling the stripe feature points and the stripe reference points, dyeing the sample, screening a local reference point according to the comparison condition of gray values after dyeing, adding compensation stirring to the raw material mixture with the local reference point in the stirring process, determining stirring parameters of the compensation stirring according to the local reference point, and obtaining the raw material mixture with the compensation stirring parameter. According to the preparation method, the stirred raw material mixture is subjected to crystallization control, pore expansion modification and surface functionalization, so that the target m-cresol adsorbent is prepared, further, the stirring state of the mixture is monitored in time in the preparation process, the stirring mode is adaptively adjusted according to different stirring states, and the structural uniformity of the m-cresol adsorbent is improved.

Description

Technical Field

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

[0002] Meta-p-cresol is an important organic chemical raw material, widely used in pesticides, medicines, spices, dyes and other fields. However, it has strong irritation and corrosiveness. If wastewater containing meta-p-cresol is discharged directly without effective treatment, it will threaten the environment and human health. The adsorption method can separate meta-p-cresol from wastewater through the physical or chemical reaction between the adsorbent and meta-p-cresol. HZSM-5 molecular sieve is a silicate material with unique pore structure and acidity. It has a large specific surface area and regular microporous structure, which can provide abundant adsorption sites. It can be transformed into a high-efficiency meta-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, in the hydrothermal synthesis process of the preparation of meta-p-cresol adsorbent, the mixing of reactants such as silicon source, aluminum source and template agent in the solution is not sufficient, which will lead to differences in local concentration and affect the structural uniformity and performance stability of the meta-p-cresol adsorbent. Therefore, timely monitoring of the stirring state and adaptive process adjustment to improve the structural uniformity of the meta-p-cresol adsorbent are technical problems that need to be solved.

[0003] For example, China Patent Application Publication No.: CN117861611A, the invention discloses a method for preparing an adsorbent for separating and purifying isomers of m-cresol. The invention discloses that the LSX molecular sieve with an Si / Al atomic ratio in the range of 1.0 to 1.1 is fully stirred and mixed with pillared bentonite and polyacrylamide, and then rolled into balls, and then exchanged with Group IA and Group IIA metal cations, and then dried, dehydrated, activated and other treatments to obtain a shaped adsorbent, which is loaded into a countercurrent simulated moving bed to achieve continuous feeding of m-cresol material and desorbent and continuous withdrawal of extract and raffinate materials, and finally obtain high-purity m-cresol and p-cresol products.

[0004] The prior art still has the following problems: The prior art does not take into account that in the process of preparing a meta-para-cresol adsorbent using HZSM-5 molecular sieve as a porous material, insufficient mixing of reactants such as a silicon source, an aluminum source and a template agent may lead to inconsistent reaction processes of various parts in the mixture, thereby 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 mode according to different stirring states, which affects the structural uniformity of the preparation of the meta-para-cresol adsorbent. Summary of the invention

[0005] To this end, the present invention provides a porous material-based meta-cresol adsorbent and a preparation method thereof, so as to overcome the problem that the prior art cannot timely monitor the stirring state of the mixture during the preparation process, cannot adaptably adjust the stirring mode according to the different stirring states, and affects the structural uniformity of the preparation of the meta-cresol adsorbent.

[0006] To achieve the above object, the present invention provides a method for preparing a m-p-cresol adsorbent based on a porous material, comprising: Mixing the raw materials required for the preparation into a raw material mixture according to preset components, and stirring the mixture; Acquire surface images of the raw material mixture at several moments within a preset acquisition period, mark stripe feature points according to stripe profiles in the surface image and determine feature stripe profiles, and acquire the quantity change of stripe feature points at each moment in time sequence to determine a sampling time window for the raw material mixture; Sampling the stripe feature points and the stripe reference points on the characteristic stripe profile in the sampling time window; The characteristic samples collected at the characteristic points of the stripes and the reference samples collected at the reference points of the stripes are dyed, and the local reference points are selected according to the gray value comparison after dyeing; Compensatory stirring is added to the raw material mixture with local reference points during the stirring process, and stirring parameters for compensatory stirring of the characteristic stripe profile are determined according to the number of local reference points on the characteristic stripe profile, including: Determine the stirring center point of the compensating stirring according to the comparison of the gray values ​​of the characteristic samples at a plurality of local reference points, and determine the stirring radius of the compensating stirring according to the interval between the stirring center point and each local reference point; Or, taking a local reference point as the stirring center point of the compensating stirring, and determining the stirring radius of the compensating stirring according to the gray value comparison at the local reference point; The stirred raw material mixture is subjected to crystallization control, pore expansion modification and surface functionalization to obtain the target m-para-cresol adsorbent.

[0007] Furthermore, the process of marking the stripe feature points and determining the feature stripe contours includes: Identify fringe discontinuities in surface images; If the tangent directions of the end points of the stripe profiles on both sides of the stripe discontinuity are the same, the stripe profiles on both sides of the stripe discontinuity are merged to determine the characteristic stripe profile, and the stripe discontinuity is marked as the stripe characteristic point.

[0008] Furthermore, the process of determining the sampling time window of the raw material mixture includes: A plurality of acquisition moments are set within a preset acquisition cycle, and the difference between the number of fringe feature points in the surface image at a later acquisition moment and the number of fringe feature points in the surface image at a previous acquisition moment is calculated respectively, and the difference is combined into a sequence in time sequence; If the number sequence is an increasing number sequence, the last acquisition time in the acquisition period is determined as the sampling time window of the raw material mixture; If the sequence is not an increasing sequence, the raw material mixture is not sampled.

[0009] 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 characteristic point.

[0010] Furthermore, the process of selecting local reference points includes: Acquire a first grayscale value of a characteristic sample collected at a stripe characteristic point after dyeing, and a second grayscale value of a reference sample collected at a stripe reference point of a characteristic stripe profile where the stripe characteristic point is located after dyeing; Calculating an absolute value of a difference between the first grayscale value and the second grayscale value, and determining the absolute value of the difference as a content characterization value of the stripe feature point; If the content characterization value of the stripe feature point meets the reference point determination condition, the stripe feature point is selected as a local reference point; The reference point determination condition is that the content characterization value exceeds a preset content reference value.

[0011] Further, the process of determining stirring parameters for compensating stirring of the characteristic stripe profile includes: If the number of local reference points on the characteristic fringe 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 between the stirring center point and each local reference point; If the number of local reference points on the characteristic fringe 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 gray value comparison at the local reference point; If the number of local reference points on the characteristic stripe profile is 0, the stirring center point and the stirring radius are not set for the characteristic stripe profile.

[0012] Furthermore, based on the determination result that the number of local reference points on the characteristic stripe profile exceeds 1, the content characterization value of each local reference point on the characteristic stripe profile is obtained, and the local reference point corresponding to the maximum content characterization value is determined as the stirring center point.

[0013] Furthermore, according to the determination result that the number of local reference points on the characteristic stripe profile exceeds 1, the interval distance between the stirring center point and the remaining local reference points is obtained, and the maximum value of the interval distance is determined as the stirring radius.

[0014] Further, 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.

[0015] The present invention also provides a porous material-based m-p-cresol adsorbent, comprising: The molar ratio of silicon dioxide to aluminum oxide is 70% to 90% in a ratio of 100:1, ferric chloride solution is 5% to 20%, and mesoporous aluminum oxide is 10% to 25%.

[0016] Compared with the prior art, the beneficial effect of the present invention lies in that the present invention mixes the raw materials required for preparation into a raw material mixture with preset components and stirs the mixture, obtains surface images of the raw material mixture at several moments within a preset acquisition period, marks stripe feature points according to the stripe profile in the surface image and determines the characteristic stripe profile, 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, samples the stripe feature points and stripe reference points on the characteristic stripe profile in the sampling time window, dyes the characteristic samples collected at the stripe feature points and the reference samples collected at the stripe reference points, selects local reference points according to the gray value comparison after dyeing, 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, performs crystallization control, pore expansion modification and surface functionalization on the raw material mixture after stirring to obtain the target m-cresol adsorbent, and further, timely monitors the stirring state of the mixture during the preparation process, adjusts the stirring mode according to the different adaptability of the stirring state, and improves the structural uniformity of the preparation of the m-cresol adsorbent.

[0017] In particular, the present invention marks stripe feature points and determines characteristic stripe profiles according to stripe profiles in the surface image. It can be understood that the stripes in the surface image of the raw material mixture are the external manifestation of its internal mixing conditions. By marking stripe feature points and determining characteristic stripe profiles, information such as the unevenness of the raw material mixing and the difference in the reaction process can be intuitively presented, and the mixing uniformity of the raw material mixture can be quantitatively evaluated. By analyzing the surface image, problems existing in the raw material mixture can be discovered in time. The present invention marks stripe feature points and determines characteristic stripe profiles through the stripe profiles in the surface image, thereby providing specific data support for quality control in the preparation process, timely monitoring the stirring state of the mixture during the preparation process, and improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0018] In particular, the present invention obtains the change in the number of stripe feature points at each moment in time series 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 the mixture and the reaction progress. By recording the change in the number in time series, the mixing state trend of the mixture can be accurately determined. Sampling at the appropriate time point can make the sample more representative, provide a reliable basis for subsequent analysis and preparation, reduce invalid sampling and avoid sampling costs and time consumption. The present invention obtains the change in the number of stripe feature points at each moment in time series to determine the sampling time window of the raw material mixture, thereby realizing timely monitoring of the stirring state of the mixture during the preparation process, improving sampling efficiency, reducing production costs, and improving the efficiency of preparation of para-cresol adsorbent.

[0019] In particular, the present invention samples the stripe characteristic points and the stripe reference points on the characteristic stripe profile in the sampling time window. It can be understood that the characteristic samples at the stripe characteristic points and the reference samples at the stripe reference points of the characteristic stripe profile where the stripe characteristic points are located both belong to the same raw material mixture on the stripe profile. By comparing the two, the component distribution state of the mixture can be more comprehensively understood, thereby improving the representativeness of the compared data. The present invention samples the stripe characteristic points and the stripe reference points on the characteristic stripe profile in the sampling time window, thereby achieving timely monitoring of the stirring state of the mixture during the preparation process and improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0020] In particular, the present invention selects local reference points according to the grayscale value comparison after dyeing. It can be understood that the stripe feature points identified by the surface image of the raw material mixture may cause misjudgment due to insufficient image recognition accuracy. The sample is dyed, and its grayscale value will vary depending on the content of the components in the sample. By comparing the grayscale values ​​of the stripe feature points and the stripe reference points, the stripe discontinuities actually existing on the surface of the mixture can be screened out to avoid misjudgment. Furthermore, it is achieved to timely monitor the stirring state of the mixture during the preparation process, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0021] 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 profile according to the number of local reference points on the characteristic stripe profile. It can be understood that compensatory stirring can make the raw material mixture at the local reference point and the surrounding area more fully exchange substances. Under the action of compensatory stirring, materials of different components around the discontinuity point are stirred up, which accelerates the molecular diffusion and convection process, so that the local reference points with composition differences can more quickly converge with the composition of the overall material, thereby improving the uniformity of the entire raw material mixture. The compensatory stirring method is determined according to the number of local reference points, which can achieve targeted stirring of the characteristic stripe profile and achieve a higher mixing uniformity in a shorter time. 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. Furthermore, it realizes timely monitoring of the stirring state of the mixture during the preparation process, and adjusts the stirring mode according to different adaptability of the stirring state, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The present invention is a logic flow chart of a method for preparing a m-p-cresol adsorbent based on porous materials according to an embodiment of the present invention; Figure 2 A logic flow chart for determining a sampling time window of a raw material mixture according to an embodiment of the present invention; Figure 3 A logic flow chart for selecting local reference points for an embodiment of the present invention; Figure 4 A logic flow chart for determining stirring parameters for compensating stirring of a characteristic fringe profile according to an embodiment of the present invention. DETAILED DESCRIPTION

[0023] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0024] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0025] It should be noted that, in the description of the present invention, terms such as "upper", "lower", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships 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 cannot be understood as a limitation on the present invention.

[0026] See also Figure 1 As shown, it is a logic flow chart of a method for preparing a meta-p-cresol adsorbent based on a porous material according to an embodiment of the present invention. The method for preparing a meta-p-cresol adsorbent based on a porous material according to the present invention comprises: Step S100, mixing the raw materials required for preparation into a raw material mixture according to preset components, and stirring; Specifically, the preset components may include 75% silicon dioxide and aluminum oxide in a molar ratio of 100:1, 10% ferric chloride solution, 10% aluminum oxide, and 5% binder. The binder may be silica sol, which will not be described in detail here.

[0027] Step S200, obtaining surface images of the raw material mixture at several moments within a preset acquisition period, marking stripe feature points according to stripe profiles in the surface image and determining feature stripe profiles, and obtaining changes in the number of stripe feature points at each moment in time sequence to determine a sampling time window for the raw material mixture; Specifically, the preset collection period can be set by those skilled in the art according to the accuracy requirements of the preparation of the m-cresol adsorbent. The higher the accuracy requirement, the longer the preset collection period. Preferably, the duration of the preset collection period can be 20 minutes.

[0028] Step S300, sampling the stripe feature points and stripe reference points on the characteristic stripe profile in the sampling time window; Specifically, the present invention samples the stripe characteristic points and the stripe reference points on the characteristic stripe profile in the sampling time window. It can be understood that the characteristic samples at the stripe characteristic points and the reference samples at the stripe reference points of the characteristic stripe profile where the stripe characteristic points are located both belong to the same raw material mixture on the stripe profile. The two can be compared to more comprehensively understand the component distribution state of the mixture and improve the representativeness of the compared data. The present invention samples the stripe characteristic points and the stripe reference points on the characteristic stripe profile in the sampling time window, thereby realizing timely monitoring of the stirring state of the mixture during the preparation process and improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0029] Specifically, the sampling amount for sampling the stripe characteristic points and the 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 technical personnel in this field according to the accuracy requirements of the preparation of the para-cresol adsorbent. The higher the accuracy requirement, 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.

[0030] Step S400, dyeing the feature samples collected at the stripe feature points and the reference samples collected at the stripe reference points, and selecting the local reference points according to the gray value comparison after dyeing; Specifically, the same amount of dye is added to the collected characteristic samples and reference samples. The dye can be silver nitrate. The amount of dye added can be set by technical personnel in this field according to the sampling amount. When the sampling amount is 20g, the value range of the added amount can be [0.05, 0.5], and the interval unit is g. If the added amount is too little, the ideal dyeing effect cannot be achieved, which makes it difficult to screen local reference points by gray value comparison. If the added amount is too much, it will cause excessive dyeing, which not only causes a waste of reagents, but also affects the subsequent observation and analysis of the samples. Preferably, the added amount can be 0.2g.

[0031] Step S500, adding compensatory stirring to the raw material mixture with local reference points during stirring, and determining stirring parameters for compensatory stirring of the characteristic stripe profile according to the number of local reference points on the characteristic stripe profile, including: Determine the stirring center point of the compensating stirring according to the comparison of the gray values ​​of the characteristic samples at a plurality of local reference points, and determine the stirring radius of the compensating stirring according to the interval between the stirring center point and each local reference point; Or, taking a local reference point as the stirring center point of the compensating stirring, and determining the stirring radius of the compensating stirring according to the gray value comparison at the local reference point; Specifically, the multi-layer nested blades can be used to drive the blades to extend and retract using hydraulic or electric push rods to achieve continuous adjustment of the stirring radius, and the offset of the eccentric shaft can be controlled by a gear rack or linear motor to adjust the stirring center, which will not be repeated here.

[0032] 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 compensatory stirring can make the raw material mixture at the local reference point and the surrounding area more fully exchange substances. Under the action of compensatory stirring, materials of different components around the discontinuity point are stirred up, which accelerates the molecular diffusion and convection process, so that the local reference points with composition differences can more quickly converge with the composition of the overall material, thereby improving the uniformity of the entire raw material mixture. The compensatory stirring method is determined according to the number of local reference points, which can achieve targeted stirring of the characteristic stripe profile and achieve a higher mixing uniformity in a shorter time. 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. Furthermore, it realizes timely monitoring of the stirring state of the mixture during the preparation process, and adjusts the stirring mode according to different adaptability of the stirring state, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0033] Step S600, performing crystallization control, pore expansion modification and surface functionalization on the stirred raw material mixture to obtain the target m-cresol adsorbent.

[0034] Specifically, at a reaction temperature of 150°C to 180°C and a reaction pressure of 0.8MPa to 1.5MPa, the reaction is carried out in a reactor for 24h to 48h for crystallization control 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 can be 1.2MPa, and the reaction time can be 30h. The non-framework aluminum of the molecular sieve is selectively dissolved by acid etching with 0.1mol / L to 0.5mol / L dilute nitric acid to generate secondary pores for pore expansion modification to improve mass transfer efficiency and alleviate micropore blockage. Preferably, the dilute nitric acid can be 0.25mol / L. By immersing in 0.5mol / L to 1.0mol / L copper sulfate solution, static ion exchange is performed at 60°C for 6h to 12h for surface functionalization to enhance adsorption selectivity and improve adsorption stability. Preferably, the copper sulfate solution can be 0.85mol / L, and the static ion exchange time can be 8h. It will not be repeated here.

[0035] Specifically, the process of marking stripe feature points and determining the feature stripe contour includes: Identify fringe discontinuities in surface images; If the tangent directions of the end points of the stripe profiles on both sides of the stripe discontinuity are the same, the stripe profiles on both sides of the stripe discontinuity are merged to determine the characteristic stripe profile, and the stripe discontinuity is marked as the stripe characteristic point.

[0036] Specifically, the surface image of the raw material mixture can be obtained by an industrial camera, and the edge algorithm can be used to identify the stripe discontinuities, stripe contours, and tangent directions of the stripe contour endpoints in the surface image. The microprocessor can be used to mark the stripe feature points and determine the feature stripe contour. This is a prior art and will not be described in detail here.

[0037] Specifically, the present invention marks stripe feature points and determines characteristic stripe profiles according to stripe profiles in the surface image. It can be understood that the stripes in the surface image of the raw material mixture are the external manifestation of its internal mixing conditions. By marking stripe feature points and determining characteristic stripe profiles, information such as the unevenness of the raw material mixing and the difference in the reaction process can be intuitively presented, and the degree of mixing uniformity of the raw material mixture can be quantitatively evaluated. By analyzing the surface image, problems existing in the raw material mixture can be discovered in a timely manner. The present invention marks stripe feature points and determines characteristic stripe profiles through the stripe profiles in the surface image, thereby providing specific data support for quality control in the preparation process, timely monitoring the stirring state of the mixture during the preparation process, and improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0038] Specifically, it reflects the stirring and mixing state. When the raw material mixture is stirred, if the stirring is uniform, the fluid should show a relatively uniform flow state, and the raw material distribution is relatively uniform. When the stirring is uneven, the velocity gradient and the uneven distribution of shear stress will be generated. In the area with large shear stress, the fluid is stretched and deformed, resulting in changes in the local concentration of the raw material. This unevenness will make the reaction process in some areas faster than in other areas, forming a striped gel. The stripe characteristic points are the discontinuities on the striped gel in the same direction. The formation of the discontinuities on the striped gel is due to the uneven distribution of the mixture. The raw material components at the discontinuities are less, and the reaction process is slower than that at the adjacent gels. Therefore, discontinuities are formed on the striped gel. The stripe characteristic points are marked by the stripe contours in the surface image and the characteristic stripe contours are determined. Furthermore, specific data support is provided for quality control in the preparation process, and the stirring state of the mixture is monitored in time during the preparation process, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0039] Specifically, see Figure 2 As shown, it is a logic flow chart of determining the sampling time window of the raw material mixture according to an embodiment of the present invention. The process of determining the sampling time window of the raw material mixture includes: A plurality of acquisition moments are set within a preset acquisition cycle, and the difference between the number of fringe feature points in the surface image at a later acquisition moment and the number of fringe feature points in the surface image at a previous acquisition moment is calculated respectively, and the difference is combined into a sequence in time sequence; If the number sequence is an increasing number sequence, the last acquisition time in the acquisition cycle is determined as the sampling time window of the raw material mixture; If the sequence is not an increasing sequence, the raw material mixture is not sampled.

[0040] In implementation, the interval length of the collection moments set within the preset collection cycle can be 2 minutes, and 10 collection moments are set. By way of example, a specific method for determining the sampling moment window of the raw material mixture is given here. If the numbers of stripe feature points in the surface image at 10 collection moments within the collection cycle are obtained as follows: 2, 3, 5, 9, 14, 21, 30, 40, 52, 65, respectively, the difference between the number of stripe feature points in the surface image at the subsequent collection moment and the number of stripe feature points in the surface image at the previous collection moment is calculated as follows: 1, 2, 4, 5, 7, 9, 10, 12, 13, respectively, and the differences are combined in time sequence into a sequence {1, 2, 4, 5, 7, 9, 10, 12, 13}, which is an increasing sequence. Therefore, the tenth collection moment is determined as the sampling moment window of the raw material mixture.

[0041] Specifically, the present invention obtains the change in the number of stripe feature points at each moment in time series 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 the mixture and the reaction progress. By recording the change in the number in time series, the mixing state trend of the mixture can be accurately determined. Sampling at the appropriate time point can make the sample more representative, provide a reliable basis for subsequent analysis and preparation, reduce invalid sampling and avoid sampling costs and time consumption. The present invention obtains the change in the number of stripe feature points at each moment in time series to determine the sampling time window of the raw material mixture, thereby realizing timely monitoring of the stirring state of the mixture during the preparation process, improving sampling efficiency, reducing production costs, and improving the efficiency of preparing the para-cresol adsorbent.

[0042] 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 the raw material mixture is stirred, the stirring device 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 materials, so that the originally unevenly distributed raw materials gradually tend to be uniform. The continuous stirring action allows the raw materials to fully contact and react on a microscopic scale, reducing local concentration differences. The number of stripe feature points will also decrease accordingly. Within the preset acquisition cycle, when the stripe feature points in the surface image at the next acquisition moment When the difference between the number of stripe feature points and the number of stripe feature points in the surface image at the previous acquisition moment is in a continuous increasing trend, it means that the number of stripe feature points does not decrease with the increase of stirring time, and the uniformity of the raw material mixture does not improve. The last acquisition moment in the preset acquisition cycle reflects the moment when the uniformity of the raw material mixture is the worst. Determining it as the sampling moment window can improve the representativeness of the sampled data. The present invention obtains the change in the number of stripe feature points at each moment in time series to determine the sampling moment window of the raw material mixture, thereby improving the representativeness of the sampled data, reducing the production cost, and improving the efficiency of the preparation of the m-cresol adsorbent.

[0043] Specifically, 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 characteristic point.

[0044] Specifically, see Figure 3 As shown, it is a logic flow chart of selecting local reference points according to an embodiment of the present invention. The process of selecting local reference points includes: Acquire a first grayscale value of a characteristic sample collected at a stripe characteristic point after dyeing, and a second grayscale value of a reference sample collected at a stripe reference point of a characteristic stripe profile where the stripe characteristic point is located after dyeing; Calculating an absolute value of a difference between the first grayscale value and the second grayscale value, and determining the absolute value of the difference as a content characterization value of the stripe feature point; Specifically, the grayscale value can be determined by obtaining a stained sample image through an industrial camera, and preprocessing the obtained sample image using an image processor. The preprocessing includes graying, filtering and denoising, and contrast enhancement. The grayscale value in the preprocessed sample image is extracted using image analysis software, which will not be repeated here.

[0045] Specifically, the grayscale value range of the first grayscale value of the feature sample collected at the stripe feature point after being dyed with silver nitrate as the dye is [100, 200], and the grayscale value range of the second grayscale value of the reference sample collected at the stripe reference point of the feature stripe profile where the stripe feature point is located after being dyed with silver nitrate as the dye is [100, 150].

[0046] If the content characterization value of the stripe feature point meets the reference point determination condition, the stripe feature point is selected as a local reference point; If the content characterization value of the stripe feature point does not meet the reference point determination condition, the stripe feature point is not screened; The reference point determination condition is that the content characterization value exceeds a preset content reference value.

[0047] Specifically, the preset content reference value can be the product of the second grayscale value and the content reference value factor. The content reference value factor can be set by technical personnel in this field according to the accuracy requirements of the preparation of para-cresol adsorbent. The higher the accuracy 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.

[0048] Exemplarily, a specific method for determining the content characterization value of a stripe feature point is given here. The first grayscale value of the characteristic sample collected at the stripe feature point after dyeing is 180, and the second grayscale value of the reference sample collected at the stripe reference point of the characteristic stripe profile where the stripe feature point is located after dyeing is 120. The absolute value of the difference between the first grayscale value and the second grayscale value is 60. Therefore, the content characterization value is 60.

[0049] Specifically, the present invention selects local reference points according to the grayscale value comparison after dyeing. It can be understood that the stripe feature points identified by the surface image of the raw material mixture may cause misjudgment due to insufficient image recognition accuracy. The sample is dyed, and its grayscale value will vary depending on the content of the components in the sample. By comparing the grayscale values ​​of the stripe feature points and the stripe reference points, the stripe discontinuities actually existing on the surface of the mixture can be screened out to avoid misjudgment. Furthermore, it is achieved to timely monitor the stirring state of the mixture during the preparation process, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0050] Specifically, there are incompletely reacted intermediates at the discontinuity points of the stripes, which contain more active sites, acidic or basic groups, and have a stronger ability to bind to metal ions, which will lead to an increase in the adsorption of metal ions at the discontinuity points. More metal ion adsorption will lead to enhanced absorption of light of a specific wavelength and a relatively weakened intensity of reflected light, resulting in a larger grayscale value. The structure and composition of the aluminosilicate precursor in the reference sample obtained at the reference point of the stripes are relatively stable, and the functional groups and charge distribution on its surface are also relatively uniform. When metal ion dyes are added, the metal ions will react with the surface of the aluminosilicate through ion exchange, coordination, etc. The specific groups are combined with the metal ions at the stripes, and due to the uniformity of the structure, the adsorption amount and distribution of the metal ions at the stripes are relatively uniform, so that the absorption and scattering of light at the stripes are relatively stable and at a lower degree. Compared with the stripe discontinuity points, it will not cause a large amount of light to be absorbed or scattered due to structural defects, uneven distribution of metal ions and other factors, so the reflected light intensity is relatively high, which is manifested as a small gray value in the imaging system. The present invention selects the actual stripe discontinuity points as local reference points through the gray value comparison after dyeing, thereby realizing timely monitoring of the stirring state of the mixture during the preparation process, and improving the structural uniformity of the preparation of the m-p-cresol adsorbent.

[0051] Specifically, see Figure 4 As shown, it is a logic flow chart of determining stirring parameters for compensating stirring of a characteristic stripe profile according to an embodiment of the present invention. The process of determining stirring parameters for compensating stirring of the characteristic stripe profile includes: If the number of local reference points on the characteristic fringe 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 between the stirring center point and each local reference point; If the number of local reference points on the characteristic fringe 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 gray value comparison at the local reference point; If the number of local reference points on the characteristic stripe profile is 0, the stirring center point and the stirring radius are not set for the characteristic stripe profile.

[0052] Specifically, under the condition that the number of local reference points on the characteristic stripe profile is 0, the present invention does not set a stirring center point and a stirring radius for the characteristic stripe profile. It can be understood that when the number of local reference points on the characteristic stripe profile is 0, in the area corresponding to the characteristic stripe profile, the composition of the raw material mixture is relatively uniform, and there are no obvious uneven points that require special treatment. Therefore, there is no need to set a stirring center point and a stirring radius to perform 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 profile where there are no local reference points more uniform. Furthermore, it is achieved that the stirring state of the mixture is monitored in time during the preparation process, and the stirring mode is adaptively adjusted according to the different stirring states, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0053] Specifically, according to the determination result that the number of local reference points on the characteristic stripe profile exceeds 1, the content characterization value of each local reference point on the characteristic stripe profile is obtained, and the local reference point corresponding to the maximum content characterization value is determined as the stirring center point.

[0054] Specifically, according to the determination result that the number of local reference points on the characteristic stripe profile exceeds 1, the interval distance between the stirring center point and the remaining local reference points is obtained, and the maximum value of the interval distance is determined as the stirring radius.

[0055] Specifically, under the condition that the number of local reference points on the characteristic stripe profile exceeds 1, the present invention determines the stirring center point of the compensatory stirring according to the comparison of the grayscale values ​​of the characteristic samples at the local reference points, and determines the stirring radius of the compensatory stirring according to the interval between the stirring center point and each local reference point. It can be understood that the comparison of the grayscale values ​​of the characteristic samples at the local reference points can reflect the difference in components in the raw material mixture. The larger the content reference value, the more significant the difference in components between the local reference point and the adjacent area. The local reference point with the largest difference is determined as the stirring center point, which can focus on stirring the area with the largest component difference, which is helpful to quickly improve The uniformity of the raw material mixture reduces the overall composition deviation. The stirring radius is determined according to the distance between the stirring center point and each local reference point, which can ensure that the stirring effect effectively covers all uneven areas that need to be improved. The stirring center is based on the distance between these points and the stirring center point. It can be ensured that during the stirring process, the areas where other local reference points are located can also be affected by the stirring effect, thereby achieving uniform mixing of the raw material mixture in the entire characteristic stripe contour area. Furthermore, it is achieved that the stirring state of the mixture is monitored in time during the preparation process, and the stirring mode is adjusted according to the different adaptability of the stirring state, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0056] 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.

[0057] 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 stirring radius value factor is too large, the stirring range will be too large, causing unnecessary energy consumption. If the value is too small, the area that needs to be stirred will not be fully covered. Preferably, the stirring radius value factor can be 0.3, the content characterization value of the local reference point is 80, the stirring radius is 24, and the unit of the stirring radius is cm.

[0058] Specifically, under the condition that the number of local reference points on the characteristic stripe profile is 1, the present invention uses the local reference point as the stirring center point of the compensatory stirring, and determines the stirring radius of the compensatory stirring according to the grayscale value comparison at the local reference point. It can be understood that when the number of local reference points is 1, this point is a significant mark of the unevenness in the raw material mixture, and it represents the position with the largest difference on the entire characteristic stripe profile. By using it as the stirring center point, stirring can be directly performed on this key area, and the local unevenness problem in the raw material mixing can be solved in a targeted manner. The content characterization value can reflect the degree of difference in composition between the 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 the purpose of homogenization. Furthermore, it is realized that the stirring state of the mixture is monitored in time during the preparation process, and the stirring mode is adjusted according to the different adaptability of the stirring state, thereby improving the structural uniformity of the preparation of the m-cresol adsorbent.

[0059] The m-p-cresol adsorbent based on porous materials of the present invention comprises: The molar ratio of silicon dioxide to aluminum oxide is 100:1, 70% to 85%, ferric chloride solution is 5% to 15%, and mesoporous aluminum oxide is 10% to 20%.

[0060] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

[0061] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing a meta-p-cresol adsorbent based on porous materials, characterized in that: include: Mixing the raw materials required for the preparation into a raw material mixture according to preset components, and stirring the mixture; Acquire surface images of the raw material mixture at several moments within a preset acquisition period, mark stripe feature points according to stripe profiles in the surface image and determine feature stripe profiles, and acquire the quantity change of stripe feature points at each moment in time sequence to determine a sampling time window of the raw material mixture; Sampling the stripe feature points and stripe reference points on the characteristic stripe profile in the sampling time window; The characteristic samples collected at the characteristic points of the stripes and the reference samples collected at the reference points of the stripes are dyed, and the local reference points are selected according to the gray value comparison after dyeing; Compensatory stirring is added to the raw material mixture with local reference points during the stirring process, and stirring parameters for compensatory stirring of the characteristic stripe profile are determined according to the number of local reference points on the characteristic stripe profile, including: Determine a stirring center point of the compensatory stirring according to a comparison of the grayscale values ​​of characteristic samples at a plurality of local reference points, and determine a stirring radius of the compensatory stirring according to a distance between the stirring center point and each local reference point; Or, taking a local reference point as the stirring center point of the compensating stirring, and determining the stirring radius of the compensating stirring according to the gray value comparison at the local reference point; The stirred raw material mixture is subjected to crystallization control, pore expansion modification and surface functionalization to obtain the target m-para-cresol adsorbent.

2. The method for preparing a meta-p-cresol adsorbent based on a porous material according to claim 1, characterized in that: The process of marking the characteristic points of the stripes and determining the characteristic stripe contours includes: Identify fringe discontinuities in surface images; If the tangent directions of the end points of the stripe profiles on both sides of the stripe discontinuity are the same, the stripe profiles on both sides of the stripe discontinuity are merged to determine the characteristic stripe profile, and the stripe discontinuity is marked as the stripe characteristic point.

3. The method for preparing a meta-p-cresol adsorbent based on a porous material according to claim 2, characterized in that: The process of determining the sampling time window of the raw material mixture includes: A plurality of acquisition moments are set within a preset acquisition cycle, and the difference between the number of fringe feature points in the surface image at a later acquisition moment and the number of fringe feature points in the surface image at a previous acquisition moment is calculated respectively, and the difference is combined into a sequence in time sequence; If the number sequence is an increasing number sequence, the last acquisition time in the acquisition period is determined as the sampling time window of the raw material mixture; If the sequence is not an increasing sequence, the raw material mixture is not sampled.

4. The method for preparing a m-p-cresol adsorbent based on a porous material according to claim 3, characterized in that: 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 characteristic point.

5. The method for preparing a m-p-cresol adsorbent based on a porous material according to claim 4, characterized in that: The process of selecting local reference points based on the gray value comparison after dyeing includes: Acquire a first grayscale value of a characteristic sample collected at a stripe characteristic point after dyeing, and a second grayscale value of a reference sample collected at a stripe reference point of a characteristic stripe profile where the stripe characteristic point is located after dyeing; Calculating an absolute value of a difference between the first grayscale value and the second grayscale value, and determining the absolute value of the difference as a content characterization value of the stripe feature point; If the content characterization value of the stripe feature point meets the reference point determination condition, the stripe feature point is selected as a local reference point; The reference point determination condition is that the content characterization value exceeds a preset content reference value.

6. The method for preparing a meta-p-cresol adsorbent based on a porous material according to claim 5, characterized in that: The process of determining stirring parameters for compensating stirring of the characteristic stripe profile includes: If the number of local reference points on the characteristic fringe 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 between the stirring center point and each local reference point; If the number of local reference points on the characteristic fringe 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 gray value comparison at the local reference point; If the number of local reference points on the characteristic stripe profile is 0, the stirring center point and the stirring radius are not set for the characteristic stripe profile.

7. The method for preparing a m-p-cresol adsorbent based on a porous material according to claim 6, characterized in that: According to the determination result that the number of local reference points on the characteristic stripe profile exceeds 1, the content characterization value of each local reference point on the characteristic stripe profile is obtained, and the local reference point corresponding to the maximum content characterization value is determined as the stirring center point.

8. The method for preparing a meta-p-cresol adsorbent based on a porous material according to claim 7, characterized in that: According to the determination result that the number of local reference points on the characteristic stripe profile exceeds 1, the interval distance between the stirring center point and the remaining local reference points is obtained, and the maximum value of the interval distance is determined as the stirring radius.

9. The method for preparing a m-p-cresol adsorbent based on a porous material according to claim 7, characterized in that: 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.

10. A m-p-cresol adsorbent based on a porous material, using the method for preparing a m-p-cresol adsorbent based on a porous material according to any one of claims 1 to 9, characterized in that: include: The molar ratio of silicon dioxide to aluminum oxide is 70% to 90% in a ratio of 100:1, ferric chloride solution is 5% to 20%, and mesoporous aluminum oxide is 10% to 25%.

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