A method and system for preparing a polymeric compound

Abstract

The application relates to the technical field of high-molecular compound preparation, and particularly relates to a high-molecular compound preparation method and system, which comprises the following steps: adding distilled water and boron nitride into a container containing silane monomers, stirring and reacting for 3-5 hours, collecting hyperspectral images of mixed solutions in the container during the stirring and reacting process, obtaining spectral similarity factors of each matching pixel in the hyperspectral images, judging the sufficient degree of the stirring and reacting according to the spectral similarity factor distribution characteristics of each pixel, completing the stirring and reacting, mixing prepared boron nitride modified silicone resin, silanol, polyester resin and crosslinking catalyst, continuously reacting for 2-4 hours at 110-130 DEG C, then adding an organic solvent, and obtaining modified polyester resin with a solid content of 62%-66%. The application aims to improve the performance and service life of the prepared modified polyester resin, and realizes a high-molecular compound preparation method.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high molecular compound preparation, in particular to a high molecular compound preparation method and system. BACKGROUND

[0002] High molecular compound is also called high molecular polymer, which generally refers to a compound with a relative molecular mass of several thousand to several million, usually connected by covalent bonds multiple times by specific structural units, and has special chemical, material and material properties. As a kind of high molecular compound, modified polyester resin has excellent metal adhesion, good physical and mechanical properties such as hardness, and good chemical corrosion resistance, while avoiding the disadvantages of polyester resin flexibility and heat resistance. It is widely used in various fields, and the modified polyester resin high molecular compound has high resistance to alkali. The structure of the high molecular compound in the alkali solution does not break down.

[0003] In the preparation step of the modified polyester resin, the silane monomer is poured into the container, distilled water and boron nitride are added, and stirring reaction is carried out. After distillation, the intermediate product of the modified polyester resin, boron nitride modified organic silicon resin, is obtained by mixing and stirring with organic solvent. In this process, the stirring reaction time needs to be strictly controlled. If the stirring reaction time is too long, the reaction may be excessive, which may cause excessive polymerization of the silane monomer during stirring and form large particles or solid precipitates, resulting in uneven boron nitride modified organic silicon resin. If the stirring reaction time is too short, the reaction may not be complete, and the silane monomer may not be fully polymerized, which may affect the hardness, heat resistance and flexibility of the modified polyester resin prepared subsequently. SUMMARY

[0004] In order to solve the above technical problems, the purpose of the present application is to provide a high molecular compound preparation method and system, and the technical scheme adopted is as follows:

[0005] In a first aspect, the present application provides a high molecular compound preparation method, which comprises the following steps:

[0006] (1) Prepare raw materials: obtain each raw material, which includes silane monomer, boron nitride, organic solvent, silanol, polyester resin, cross-linking catalyst and distilled water;

[0007] (2) Prepare boron nitride modified organic silicon resin: add distilled water and boron nitride to the container containing silane monomer, and stir at 200 230℃ for 3 5h, then cool, distill, add organic solvent and stir to obtain boron nitride modified organic silicon resin;

[0008] (3) Preparation of modified polyester resin: The boron nitride modified organosilicon resin prepared in step (2) is mixed with crosslinking catalyst, silanol and polyester resin, and then heated at 110 °C. The reaction continued at 130℃ for 2 days. After 4 hours, organic solvent was added to obtain a solid content of 62%. 66% modified polyester resin;

[0009] In step (2), during the preparation of boron nitride modified organosilicon resin, the stirring reaction was collected at equal intervals for 3 minutes. Hyperspectral images of the mixed solution in the container during the 5-hour process were collected. The first hyperspectral image was used as the initial stirring image, and all other hyperspectral images were used as reaction images. The reflection intensity of each pixel in the initial stirring image was obtained based on the significance of the reflection characteristics of each pixel. The reflection intensity of all pixels in the initial stirring image was used to obtain the segmentation threshold using a threshold segmentation algorithm. Pixels with reflection intensity greater than the segmentation threshold were recorded as feature pixels. Pixels at the locations of feature pixels in all reaction images were recorded as matching pixels. The spectral similarity factor of each matching pixel in the reaction image was obtained based on the relationship between feature pixels and matching pixels. The stirring time was controlled based on the distribution characteristics of the spectral similarity factor of each pixel.

[0010] Preferably, the silane monomer is:

[0011] The product comprises at least one of methyltrimethoxysilane, dimethyldimethoxysilane, phenyltrimethoxysilane, dimethyltrimethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane; the boron nitride is aminodichloroborane or dimethylamineborane; the organic solvent is at least one of xylene, butanol, toluene, and propylene glycol methyl ether acetate; and the crosslinking catalyst is tetrabutyl titanate or dibutyltin dilaurate.

[0012] Preferably, the amounts of silane monomer, boron nitride, distilled water, and organic solvent used in step (2) are: 58-67% silane monomer, 3-10% boron nitride, 11-12% distilled water, and 19-20% organic solvent by mass percentage.

[0013] Preferably, step (2) cooling specifically involves cooling to 65°C~75°C.

[0014] Preferably, in step (3), the mass ratio of boron nitride-modified organosilicon resin, silanol, polyester resin, and crosslinking catalyst is 1:(0.1). 0.18):(0.2 0.55): (0.01) 0.03).

[0015] Preferably, the initial stirring image is obtained according to the reflection feature intensity of each pixel, and the reflection feature intensity of each pixel in the initial stirring image is obtained according to the reflection feature prominence degree of each pixel.

[0016] The reflection difference factor of each pixel is calculated, and a neighborhood difference sequence and a neighborhood feature difference sequence of each pixel are constructed, and the expression of the reflection feature intensity of each pixel in the initial stirring image is:

[0017]

[0018] In the formula, is the reflection feature intensity of the i-th pixel in the initial stirring image, is the information entropy of the neighborhood feature difference sequence of the i-th pixel in the initial stirring image, is the total number of neighborhood paths in the pixel window of the i-th pixel in the initial stirring image, , respectively represent the neighborhood difference sequence of the x-th and y-th neighborhood path in the pixel window of the i-th pixel in the initial stirring image, represents the cosine similarity, and respectively represent the maximum reflection difference factor and the average reflection difference factor of all neighborhood pixels in the pixel window of the i-th pixel in the initial stirring image, is a natural constant, is a preset second adjustment parameter.

[0019] Preferably, the reflection difference factor of each pixel is calculated, and a neighborhood difference sequence and a neighborhood feature difference sequence of each pixel are constructed, and the expression of the reflection feature intensity of each pixel in the initial stirring image is:

[0020] For the initial stirring image, the maximum reflection band of each pixel is taken as the maximum reflection band of each pixel, the band with the highest occurrence frequency of the maximum reflection band of all pixels is taken as the significant reflection band, and the reflectivity of each pixel at the significant reflection band is taken as the significant reflectivity of each pixel.

[0021] A pixel window is constructed with each pixel as the center, 8-neighbor directions of the center pixel in the pixel window are taken as each neighborhood path of the center pixel, all pixels on the neighborhood path are taken as neighborhood pixels, a square window is constructed with each neighborhood pixel as the center, and the significant reflectivity of all pixels in the square window is constructed into a reflection matrix of each neighborhood pixel according to the position of the pixel.

[0022] The reflection matrix of each neighborhood pixel and the previous neighborhood pixel on the neighborhood path is taken as the input of the ANOSIM analysis algorithm, and the output is the global R value and the significance level value of each neighborhood pixel.

[0023] The sum of the significance level value of each neighborhood pixel and a preset first adjustment parameter is calculated, the ratio of the global R value of each neighborhood pixel to the sum is calculated, the mean of the significant reflectivity of all neighborhood pixels on the neighborhood path is calculated, the absolute value of the difference between the significant reflectivity of each neighborhood pixel and the mean is calculated, the product of the absolute value and the ratio is taken as the reflectance difference factor of each neighborhood pixel, the reflectance difference factors of all neighborhood pixels on each neighborhood path in the pixel window are arranged in order from near to far according to the distance between the neighborhood pixels and the central pixel, and the reflectance difference factors of all neighborhood pixels on each neighborhood path in the pixel window of each pixel are sorted in order from large to small as the neighborhood feature difference sequence of each pixel.

[0024] Preferably, the spectral similarity factor of each matching pixel in the reaction image is obtained according to the relationship between the feature pixel and the matching pixel, and the spectral similarity factor comprises:

[0025] The Chameleon chameleon clustering algorithm is used to obtain the clustering cluster of each pixel in the initial stirring image and the clustering cluster of each matching pixel in each reaction image.

[0026] For each matching pixel in the reaction image at each acquisition time, the spectral vector angle between the matching pixel and the feature pixel at the corresponding position is calculated, denoted as the first spectral vector angle, the spectral vector angle between the matching pixel and the matching pixel at the corresponding position in the reaction image at the previous acquisition time is calculated, denoted as the second spectral vector angle, and the sum of the first spectral vector angle and the second spectral vector angle is calculated, denoted as the first sum.

[0027] The absolute value of the difference between the mean of the significant reflectivity of the feature pixel corresponding to each matching pixel in the clustering cluster of the initial stirring image and the mean of the significant reflectivity of all pixels in the clustering cluster of the reaction image is calculated, denoted as the first absolute difference, the absolute value of the difference between the mean of the significant reflectivity of all pixels in the clustering cluster of the reaction image and the mean of the significant reflectivity of all pixels in the clustering cluster of the matching pixel at the corresponding position in the reaction image at the previous acquisition time is calculated, denoted as the second absolute difference, and the sum of the first absolute difference and the second absolute difference is calculated, denoted as the second sum. The ratio of the first sum to the second sum is taken as the spectral similarity factor of each matching pixel in the reaction image.

[0028] Preferably, the control stirring time comprises:

[0029] presetting an adjustment interval, sorting the spectral similarity factors of each matching pixel in the adjustment interval at all acquisition time instants in time sequence order as a spectral similarity sequence of each matching pixel, arranging the spectral similarity sequences of all matching pixels in the adjustment interval in rows to construct a spectral similarity matrix, and using an STL sequence decomposition algorithm to obtain the trend items of the elements in each spectral similarity sequence in each adjustment interval;

[0030] The expression of the reaction change persistence factor of each matching pixel in each adjustment interval is:

[0031]

[0032] In the formula, denotes the reaction change persistence factor of the fth matching pixel in the zth adjustment interval, and respectively denote the maximum spectral similarity factor, the minimum spectral similarity factor and the mean value of all spectral similarity factors in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval; is the total number of elements in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, is the trend item intensity of the mth element in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval;

[0033] The expression of the stirring reaction stability characteristic coefficient of each adjustment interval is:

[0034]

[0035] In the formula, is the stirring reaction stability characteristic coefficient of the zth adjustment interval, is the total number of matching pixels, is the information entropy of all elements in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, respectively denote the spectral similarity matrices of the zth and z-1th adjustment intervals, is the Euclidean distance, and norm is a normalization function;

[0036] A stirring reaction time threshold value is preset, if the stirring reaction stability characteristic coefficient of the adjustment interval is less than the stirring reaction time threshold value, the stirring reaction time of one adjustment interval is increased, otherwise, the stirring reaction is stopped.

[0037] In a second aspect, the embodiments of the present application also provide a high polymer compound preparation system, which comprises a memory, a processor and a computer program stored in the memory and running on the processor, and the processor implements the steps of the method in any of the above aspects when executing the computer program.

[0038] The present application has at least the following beneficial effects:

[0039] The application obtains the reflection feature intensity of each pixel by the initial stirring image of the reflectivity difference feature, identifies the feature pixels and matching pixels according to the reflection feature intensity, avoids the analysis of all pixels in the high spectrum image of the stirring solution, determines the pixels with significant reflectivity change features in the neighborhood range on the basis of saving the computing resources, and can more accurately evaluate the fullness of the stirring reaction. The spectral similarity factor is constructed between the spectral features of the feature pixels and the matching pixels, the stirring reaction feature stability coefficient based on the adjustment interval is obtained according to the change condition of the spectral feature similarity degree of all matching pixels in the adjustment interval, the change duration and the reaction stability feature of the spectral similarity degree of all matching pixels in the adjustment interval are comprehensively considered, the fullness of the stirring reaction in the adjustment interval can be more accurately measured, and the stirring reaction time is adjusted based on this, the stirring reaction time can be adaptively adjusted according to the features of the stirring solution in the adjustment interval, and then the boron nitride modified organic silicon resin with better performance is obtained, the modified polyester resin with better heat resistance and mechanical properties is prepared, and the alkali resistance of the modified polyester resin is improved. BRIEF DESCRIPTION OF DRAWINGS

[0040] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art and the advantages thereof, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained without creative labor based on these drawings.

[0041] Figure 1 A step flow chart of a high polymer compound preparation method provided by an embodiment of the present application is shown in the figure.

[0042] Figure 2 An adjustment stirring reaction time flow chart is shown in the figure.

[0043] Figure 3 A modified polyester resin preparation flow chart is shown in the figure.

[0044] Figure 4 A Chameleon cluster result image of the initial stirring image is shown in the figure. DETAILED DESCRIPTION

[0045] In order to further clarify the technical means and effects taken by the present application to achieve the predetermined inventive objectives, the following describes in detail the specific implementation, structure, features and effects of a high polymer compound preparation method and system according to the present application, in combination with the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. In addition, the specific features, structures or characteristics in one or more embodiments can be combined in any suitable form.

[0046] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.

[0047] The following describes in detail the specific scheme of a high polymer compound preparation method and system provided by the present application.

[0048] Preparation of polyester resin:

[0049] Ternary alcohol: 134 g of trimethylolpropane; dihydric alcohol: 10.4 g of neopentyl glycol; 107.9 g of isophthalic acid; 6.7 g of xylene; organic solvent: 200 g of propylene glycol methyl ether acetate.

[0050] After mixing 134 g of trimethylolpropane and 10.4 g of neopentyl glycol uniformly, heating to 80°C, then adding 107.9 g of isophthalic acid and 6.7 g of xylene; after heating at 200°C for 2 h, increasing the temperature to 230°C, heating for 2 h, then decreasing the temperature to 90°C, adding 200 g of propylene glycol methyl ether acetate, the polyester resin in each embodiment is obtained.

[0051] Example 1

[0052] Please refer to Figure 1 which shows a step flowchart of a high polymer compound preparation method provided by this embodiment, which includes the following steps:

[0053] Step S001, obtaining the preparation raw materials of the modified polyester resin.

[0054] (1) Preparation of raw materials

[0055] Silane monomer: methyltrimethoxysilane, dimethyldimethoxysilane, phenyltrimethoxysilane;

[0056] Boron nitride: aminodichloroborane; organic solvent: xylene, propylene glycol methyl ether acetate;

[0057] Silanol: KR220L solid silanol, weight average molecular weight of 850, hydroxyl content of 3% 5w%;

[0058] Polyester resin: polyester resin obtained in the synthesis example; crosslinking catalyst (tetrabutyl titanate); distilled water.

[0059] (2) Preparation of boron nitride-modified silicone resin

[0060] The silane monomers: 3.72 g of methyltrimethoxysilane, 2.4 g of dimethyldimethoxysilane, and 1.99 g of phenyltrimethoxysilane were mixed and poured into a four-necked flask equipped with a condenser, a stirrer, a thermometer, and an addition funnel. 1.34 g of distilled water and 0.5 g of aminoborane dichloride were slowly added to the four-necked flask, and the stirrer was turned on and stirred at 200°C for 3 h 5 h. After cooling to 75°C, distillation was performed to remove low-boiling small molecules, and then 2.3 g of an organic solvent, xylene, was poured into the four-necked flask. After uniform mixing and stirring, an emulsion was obtained, and a boron nitride-modified silicone resin was obtained.

[0061] (3) Preparation of modified polyester resin

[0062] The polyester resin 70 g obtained in the synthesis example, the silanol 23 g, the boron nitride-modified silicone resin 230 g, and tetrabutyl titanate 2.3 g were mixed, and then propylene glycol methyl ether acetate 50 g was added after continuous reaction at 110°C for 2 h. The heating and stirring were stopped, and the temperature was lowered to obtain a modified polyester resin with a solid content of 62%.

[0063] Example 2

[0064] (1) Preparation of raw materials

[0065] Silane monomers: dimethyltrimethoxysilane, phenyltrimethoxysilane;

[0066] Boron nitride: aminoborane dichloride; organic solvent: toluene, propylene glycol methyl ether acetate;

[0067] Silanol: KR220L solid silanol with a weight average molecular weight of 850 and a hydroxyl content of 3% 5 w%;

[0068] Polyester resin: polyester resin obtained in the synthesis example; crosslinking catalyst (dibutyltin dilaurate); distilled water.

[0069] (2) Preparation of boron nitride-modified silicone resin

[0070] The silane monomers: 6 g of dimethyltrimethoxysilane, 1.99 g of phenyltrimethoxysilane were mixed and poured into a four-necked flask equipped with a condenser, a stirrer, a thermometer, and an addition funnel. 1.61 g of distilled water and 0.8 g of aminoborane dichloride were slowly added to the four-necked flask, and the stirrer was turned on and stirred at 230°C for 3 h 5h. Distillation was performed after cooling to 65°C to distill off low-boiling small molecules, and then 2.68 g of the organic solvent toluene was poured into the four-necked flask. After mixing and stirring, an emulsion was obtained, and a boron-nitrogen modified silicone resin was obtained.

[0071] (3) Preparation of modified polyester resin

[0072] The polyester resin 92 g obtained in the synthesis example, the silanol 34 g, the boron-nitrogen modified silicone resin 230 g, and dibutyltin dilaurate 3 g were mixed, and then propylene glycol methyl ether acetate 40 g was added after continuous reaction at 120°C for 3 h. Heating and stirring were stopped, and the product was discharged after cooling, to obtain a modified polyester resin with a solid content of 64%.

[0073] Example 3

[0074] (1) Preparation of raw materials

[0075] Silane monomer: methyltriethoxysilane, dimethyldiethoxysilane;

[0076] Boron-nitrogen compound: aminodichloroborane; organic solvent: butanol, propylene glycol methyl ether acetate;

[0077] Silanol: KR220L solid silanol with a weight average molecular weight of 850 and a hydroxyl content of 3% 5w%;

[0078] Polyester resin: polyester resin obtained in the synthesis example; crosslinking catalyst (tetra-n-butyl titanate); distilled water.

[0079] (2) Preparation of boron-nitrogen modified silicone resin

[0080] The silane monomers 3.56 g of methyltriethoxysilane and 2.96 g of dimethyldiethoxysilane were mixed and poured into a four-necked flask equipped with a condenser, a stirrer, a thermometer, and an addition funnel. 1.22 g of distilled water and 1.1 g of dimethylamine borane were slowly added to the four-necked flask, and the stirrer was turned on. The mixture was stirred at 210°C for 3 h. 5h. Distillation was performed after cooling to 70°C to distill off low-boiling small molecules, and then 2.1 g of the organic solvent butanol was poured into the four-necked flask. After mixing and stirring, an emulsion was obtained, and a boron-nitrogen modified silicone resin was obtained.

[0081] (3) Preparation of modified polyester resin

[0082] The polyester resin 120 g obtained in the synthesis example, the silanol 40 g, the boron-nitrogen modified silicone resin 230 g, and tetra-n-butyl titanate 6 g were mixed, and then propylene glycol methyl ether acetate 30 g and butanol 20 g were added after continuous reaction at 120°C for 3 h. Heating and stirring were stopped, and the product was discharged after cooling, to obtain a modified polyester resin with a solid content of 66%.

[0083] The mixing solution in the stirring reaction process in the preparation stage of the boron-nitride modified organosilicon of each embodiment is imaged by a hyperspectral imager, and the imaging starts at the beginning of the stirring reaction. The imaging time interval is 1 min, which can be set by the implementer according to the actual situation, and the embodiment does not limit this. The hyperspectral image is collected at a top view angle. In order to avoid the loss of image details caused by the existence of much noise in the hyperspectral image of the stirring solution, the hyperspectral image obtained needs to be preprocessed. The mean filtering algorithm is used to denoise the hyperspectral image of the stirring solution. The mean filtering algorithm is a known technology, and the embodiment does not make a detailed description here. The implementer can select other algorithms to denoise the hyperspectral image of the stirring solution according to the actual situation.

[0084] At this point, the time-based stirring solution hyperspectral image can be obtained. The first stirring solution hyperspectral image collected is recorded as an initial stirring image, and all the subsequent stirring solution hyperspectral images collected are recorded as reaction images.

[0085] In step S002, the reflectance feature intensity of each pixel is obtained based on the reflectance difference feature in the initial stirring image. The feature pixel and the matching pixel are determined based on the reflectance feature intensity. The spectral similarity factor is constructed based on the spectral features of the feature pixel and the matching pixel. The stirring reaction feature stability coefficient based on the adjustment interval is obtained based on the change condition of the spectral feature similarity degree of all the matching pixels in the adjustment interval, and the stirring reaction time is adjusted based on the stirring reaction feature stability coefficient.

[0086] Specifically, in this embodiment, the silane monomer is first poured into a container, distilled water and boron-nitride are added, and the stirring reaction is performed for 3 5 hours. The hyperspectral image of the mixed solution in the container during the stirring reaction is collected. The spectral similarity factor of each matching pixel in the hyperspectral image is obtained. The degree of completion of the stirring reaction is determined based on the spectral similarity factor distribution characteristics of each pixel. The stirring reaction is completed. The boron-nitride modified organosilicon resin, the silanol, the polyester resin, and the cross-linking catalyst prepared are mixed in the container, and the mixture is reacted at 110 130℃ for 2-4h. The organic solvent is added to obtain a modified polyester resin with a solid content of 62% 66%. The stirring reaction time adjustment process is shown in the figure Figure 2 . The modified polyester resin preparation process is shown in the figure Figure 3 . The construction process of the stirring reaction stability characteristic coefficient of each adjustment interval is as follows:

[0087] When the difference between the reflectivity of a pixel and the surrounding environment is larger in the initial stirring image, the more sufficient the stirring reaction can be measured according to the spectral feature change condition of the pixel during the stirring reaction of the silane monomer, distilled water and boron nitride; secondly, when the difference between the reaction image and the initial stirring image continues to change, it indicates that the stirring reaction is still in progress, and the stirring reaction time needs to be appropriately prolonged, so that the reaction between the silane monomer, distilled water and boron nitride is more sufficient, and the initial stirring image is analyzed.

[0088] The maximum wavelength band of the reflectivity of each pixel in the initial stirring image is taken as the maximum reflection wavelength band of each pixel, the wavelength band with the highest occurrence frequency among the maximum reflection wavelength bands of all pixels in the initial stirring image is taken as the significant reflection wavelength band of the initial stirring image, and the reflectivity of each pixel in the significant reflection wavelength band in the initial stirring image is taken as the significant reflectivity of each pixel, denoted as a.

[0089] A pixel window is constructed with each pixel in the initial stirring image as the center, the size of the pixel window is 7*7, the eight neighborhood direction paths of each center pixel in the pixel window are respectively denoted as the neighborhood paths of the center pixel, the pixels on all neighborhood paths in the pixel window are denoted as neighborhood pixels, a feature window is constructed with all neighborhood pixels in the pixel window as the center, the size of the feature window is 3*3, and a reflection matrix of the neighborhood pixels is constructed according to the significant reflectivity of all pixels in the feature window of each neighborhood pixel according to the position of the pixel.

[0090] Now taking the jth neighborhood pixel on the xth neighborhood path in the ith pixel window as an example, the reflection matrices of the jth neighborhood pixel and the previous neighborhood pixel on the neighborhood path are taken as inputs, the ANOSIM (Analysis of similarities) analysis method is used to obtain the global R value and the significance level value p between the two reflection matrices, in order to highlight the reflectivity difference characteristics between each neighborhood pixel and the previous neighborhood pixel on the neighborhood path, the obtained global R value and the significance level value p are assigned to the jth pixel on the neighborhood path, wherein the larger the global R value, the larger the difference between the two reflection matrices, and the smaller the significance level value p, the more significant the difference. The ANOSIM analysis method is a known technology, and this embodiment will not be described in detail.

[0091] Based on the above analysis, a reflection difference factor is constructed to represent the significant degree of the reflection feature of each pixel in the initial stirring image, and the expression is:

[0092]

[0093] In the formula, is the reflection difference factor of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, the global R value of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, the significance level value p of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, the significant reflectance of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, the average significant reflectance of all neighborhood pixels on the xth neighborhood path of the ith pixel in the initial stirring image; a preset first adjustment parameter, to prevent a situation where the denominator is 0, in the present embodiment , the implementer can set it according to actual conditions, and the present embodiment does not limit this.

[0094] When the ratio of the global R value and the significance level value of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image is larger, that is, larger, it indicates that the difference between the corresponding reflection matrix of the neighborhood pixel and the previous neighborhood pixel on the neighborhood path is larger; at the same time, when the absolute value of the difference between the significant reflectance of the neighborhood pixel and the average significant reflectance of all neighborhood pixels on the neighborhood path is larger, that is, larger, it indicates that the difference between the significant reflectance of the neighborhood pixel and the average significant reflectance on the neighborhood path is larger, and the reflectance feature difference between the corresponding position of the neighborhood pixel and the surrounding environment is larger, and the reflection difference factor is larger.

[0095] The reflection difference factors of all neighborhood pixels on each neighborhood path in the pixel window are constructed in the order of the distance from the center pixel, and the neighborhood difference sequence of each neighborhood path is recorded as The reflection difference factors of each neighborhood pixel on all neighborhood paths in the pixel window of the center pixel are constructed in the order from large to small, and the neighborhood feature difference sequence of the center pixel is recorded as c, if the reflection difference factors are equal, then the neighborhood feature difference sequence of the center pixel is constructed in the order of the distance from the center pixel, and the expression of the reflection feature intensity of each pixel in the initial stirring image is:

[0096]

[0097] In the formula, is the reflection feature intensity of the ith pixel in the initial stirring image, is the information entropy of all elements in the neighborhood feature difference sequence of the ith pixel in the initial stirring image, is the total number of neighborhood paths in the pixel window of the ith pixel in the initial stirring image, a neighborhood difference sequence of an xth neighborhood path in a pixel window of an ith pixel in the initial stirring image, a neighborhood difference sequence of a yth neighborhood path in the pixel window of the ith pixel in the initial stirring image, a cosine similarity between a maximum reflection difference factor of all neighborhood pixels in the pixel window of the ith pixel in the initial stirring image, a mean reflection difference factor of all neighborhood pixels in the pixel window of the ith pixel in the initial stirring image, a cosine similarity between a maximum reflection difference factor of all neighborhood pixels in the pixel window of the ith pixel in the initial stirring image, a cosine similarity between a preset second adjustment parameter, to prevent the denominator from being 0, in the embodiment , the implementer can set it according to the actual situation, and the embodiment does not limit it.

[0098] When the information entropy of the neighborhood feature reflection sequence corresponding to the ith pixel in the initial stirring image is larger, that is, , the reflection difference factor fluctuation condition of each neighborhood pixel in the neighborhood range of the pixel is larger; at the same time, when the sum of the cosine similarities between the neighborhood difference sequences corresponding to all neighborhood paths in the pixel window of the ith pixel in the initial stirring image is smaller, that is, , the reflection difference conditions of the neighborhood pixels on each neighborhood path in the pixel window are less similar; at the same time, when the difference between the maximum reflection difference factor and the mean reflection difference factor of all neighborhood pixels in the pixel window is larger, that is, , the maximum reflection difference condition and the average reflection difference condition in the neighborhood range of the pixel are more different, the reflectance difference feature in the neighborhood range of the position corresponding to the pixel is more significant, and the pixel should be used as a feature pixel for subsequent analysis, that is, the reflection feature intensity is larger.

[0099] All the reflection feature intensities of all the pixels in the initial stirring image are arranged in ascending order to construct a reflection feature intensity sequence, the reflection feature intensity sequence is taken as input, the OTSU method is used to obtain a segmentation threshold of the reflection feature intensity sequence, and the pixels with a reflection feature intensity greater than the segmentation threshold are recorded as feature pixels . The pixels at positions of the feature pixels in all the reaction images are recorded as matching pixels all feature pixels in the initial stirring image are taken as nodes of an undirected graph, the absolute value of the difference between the reflected feature intensities of the nodes is taken as a distance measurement manner, and the Chameleon chameleon clustering algorithm is used to obtain each clustering cluster in the initial stirring image, denoted as k. Similarly, each matching pixel in the reaction image at each collection time is taken as a node of an undirected graph, the absolute value of the difference between the reflected feature intensities of the nodes is taken as a distance measurement manner, and the Chameleon chameleon clustering algorithm is used to obtain each clustering cluster in the reaction image at each collection time, denoted as g. The Chameleon chameleon clustering algorithm is a known technology, and will not be described in detail in this embodiment. The Chameleon chameleon clustering result image of the initial stirring image is shown in FIG. 8. Figure 4

[0100] The spectral vector included angle between pixels is obtained by SAM (Spectral Angle Mapper) spectral angle mapping, denoted as Ab. Since the SAM spectral angle mapping is a known technology, it will not be described in detail in this embodiment. Based on the above analysis, a spectral similarity factor is constructed, and the expression is as follows:

[0101]

[0102] In the formula, is the spectral similarity factor of the f th matching pixel in the reaction image at the t th collection time, is the f th matching pixel in the reaction image at the t th collection time, is the f th matching pixel in the reaction image at the t-1 th collection time, is the f th feature pixel in the initial stirring image, is the spectral vector included angle between the pixels and ; and is the spectral vector included angle between the pixels and . is the average albedo of all pixels in the clustering cluster to which the f th feature pixel in the initial stirring image belongs; is the average albedo of all pixels in the clustering cluster to which the f th matching pixel in the reaction image at the t th collection time belongs, is the average albedo of all pixels in the clustering cluster to which the f th matching pixel in the reaction image at the t-1 th collection time belongs.

[0103] When the sum of the spectral vector included angle between the f th feature pixel in the initial stirring image and the f th matching pixel in the reaction image at the t th collection time and the spectral vector included angle between the f th matching pixel in the reaction image at the t th and t-1 th collection times is smaller, that is, ​The smaller, the higher the degree of spectral feature matching between the pixels; meanwhile, when the absolute value of the difference between the mean of the significant reflectance of all pixels in the cluster to which the fth feature pixel in the initial stirring image belongs and the mean of the significant reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the tth moment belongs, and the sum of the absolute values of the difference between the mean of the significant reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the tth and t-1th moments belongs is smaller, that is, The smaller, the smaller the difference in significant reflectance between the clusters to which the pixels belong, the more similar the spectral features of the pixel at the tth moment to the corresponding positions in the initial stirring image and the reaction image at the t-1th moment, and the larger the spectral similarity factor .

[0104] Each 30 min is recorded as an adjustment interval. Taking the zth adjustment interval as an example, the spectral similarity sequence of the pixel is constructed according to the spectral similarity factors of each matching pixel in the zth adjustment interval in chronological order, denoted as H. The spectral similarity sequence of all matching pixels in the adjustment interval is constructed as a row to construct the spectral similarity matrix of the adjustment interval, denoted as V. The trend item intensity of each element in the spectral similarity sequence of all matching pixels in the zth adjustment interval is obtained by the STL sequence decomposition algorithm (Seasonal-Trend decomposition using LOESS), denoted as Since the STL sequence decomposition algorithm is a known technology, this embodiment will not be described in detail.

[0105] Based on the above analysis, the stirring reaction feature stability coefficient is constructed to represent the degree of sufficiency of the stirring reaction in the adjustment interval, and the expression is:

[0106]

[0107]

[0108] In the formula, represents the reaction change persistence factor of the fth matching pixel in the zth adjustment interval, represents the maximum spectral similarity factor in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, represents the minimum spectral similarity factor in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, is the mean of all spectral similarity factors in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, is the total number of elements in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, The trend item intensity of the mth element in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval is denoted as , which can be set by the implementer according to actual conditions, and embodiments of the present application do not limit this;

[0109] The stirring reaction stability characteristic coefficient of the zth adjustment interval is denoted as , which is the total number of matching pixels, The information entropy of all elements in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval is denoted as , which represents the spectral similarity matrix of the zth adjustment interval, , which represents the spectral similarity matrix of the (z-1)th adjustment interval, , which is the Euclidean distance between the matrices and , and norm is a normalization function, so that the value range of is within the range of [0, 1].

[0110] When the difference between the maximum and minimum spectral similarity factors in the spectral similarity sequence corresponding to the fth matching pixel in the zth adjustment interval is larger, that is, , it indicates that the spectral similarity factor of the matching pixel changes more in the adjustment interval, and the stirring reaction in the adjustment interval is more sufficient; at the same time, when the mean of all spectral similarity factors in the spectral similarity sequence is smaller, that is, , it indicates that the spectral similarity degree of the matching pixel at each collection time in the adjustment interval is smaller; at the same time, when the sum of the trend item intensities of all elements in the spectral similarity sequence is larger, that is, , it indicates that the change of the spectral similarity factor of the matching pixel in the adjustment interval is more obvious, and the change of the stirring reaction at the position corresponding to the matching pixel is more significant, and the reaction change persistence factor is larger.

[0111] When the sum of the product of the reaction change persistence factor of all matching pixels in the zth adjustment interval and the information entropy of the spectral similarity sequence of all matching pixels in the adjustment interval is larger, that is, , it indicates that the reaction change persistence of the spectral similarity factor of all matching pixels in the adjustment interval is more significant, and the stirring reaction at the position corresponding to all matching pixels in the adjustment interval is more likely to be in the process, so the stirring reaction time should be extended at this time to make the stirring reaction proceed sufficiently; at the same time, when the Euclidean distance between the spectral similarity matrices of the zth adjustment interval and the previous adjustment interval is smaller, that is, The smaller, the smaller the difference between the spectral similarity factors of all matching pixels in the two adjustment intervals, the more stable the stirring reaction of all matching pixels in the zth adjustment interval, and the more the stirring reaction time should be prolonged, so that the stirring reaction is fully carried out, that is, the stirring reaction stability characteristic coefficient The larger, the more stable the stirring reaction.

[0112] At this point, the stirring reaction stability characteristic coefficient of each adjustment interval can be obtained, and the stirring time threshold value is set In the embodiment , the implementer can set it according to the actual situation, and the embodiment does not limit it. When the stirring reaction characteristic coefficient of the adjustment interval is less than the stirring time threshold value , the stirring reaction time of one adjustment interval is increased, that is, the stirring time is prolonged by 30 min; otherwise, when the stirring reaction characteristic coefficient of the adjustment interval is greater than or equal to the stirring time threshold value , the stirring reaction is stopped.

[0113] At this point, the optimal stirring reaction time of each embodiment can be obtained by the above-mentioned manner, and then the intermediate product with less large particles or solid precipitate and fully polymerized silane monomer can be obtained, and the boron nitride modified silicone resin with good performance and high alkali resistance can be obtained according to the preparation method, which is used for the preparation of modified polyester resin.

[0114] Step S003, preparing a modified polyester resin according to the obtained boron nitride modified silicone resin with fully stirred reaction, and testing the performance of the modified polyester resin.

[0115] The performance of the obtained modified polyester resin is tested, specifically as follows:

[0116] Thermogravimetric analysis: tested by using a thermogravimetric analyzer, under high-purity nitrogen atmosphere, the heating rate is set to 10℃ / min.

[0117] Heat resistance analysis: coat the resin modified by polyester on the treated test piece, put the test piece into the constant temperature oven of the potentiometer after baking at 280℃ for 10 min, increase the temperature at 5℃ / min, start timing when the furnace temperature reaches the required temperature, take out the sample after continuous high temperature, cool to room temperature (25℃), and observe the surface condition of the coating with a magnifying glass. If there is no cracking or falling phenomenon, it means that the coating has good heat resistance.

[0118] Adhesion test: tested according to GB / T9286-1998.

[0119] Determination of paint film impact strength: tested according to GB / T1732-93.

[0120] Paint film flexibility test: tested according to GB / T1731-39.

[0121] The performance test results of the modified polyester resin are shown in Table 1.

[0122] Table 1 Performance test table

[0123]

[0124] So far, the polymer compound preparation method and system can be realized according to the above method.

[0125] Based on the same inventive concept as the above method, the embodiments of the present application also provide a polymer compound preparation system, comprising a memory, a processor and a computer program stored in the memory and running on the processor, wherein the processor implements the steps of any one of the above polymer compound preparation methods when executing the computer program.

[0126] To sum up, the embodiments of the present application comprehensively consider the change duration and reaction stability characteristics of the spectral similarity degree of all matching image elements in the adjustment interval, can more accurately measure the sufficient condition of the stirring reaction in the adjustment interval, and take it as the basis for adjusting the stirring reaction time, can adaptively adjust the stirring reaction time according to the characteristics of the stirring solution in the adjustment interval, and then obtain a boron nitride modified organic silicon resin with good performance, and finally obtain a modified polyester resin with good heat resistance and mechanical properties.

[0127] It should be noted that the above-mentioned sequence of the embodiments of the present application is only for description, and does not represent the advantages and disadvantages of the embodiments. And the above describes the specific embodiments of the present application. In addition, the processes depicted in the drawings do not necessarily require the specific order or continuous order shown to achieve the desired results. In some embodiments, multi-task processing and parallel processing are also possible or may be advantageous.

[0128] Each embodiment in the present specification is described in a progressive manner, and the same or similar parts between each embodiment can be referred to each other, and each embodiment mainly describes the difference from other embodiments.

[0129] The above only describes the preferred embodiments of the present application, and does not limit the present application, any modification, equivalent replacement, improvement, etc. made within the principles of the present application shall be included in the protection scope of the present application.

Claims

1. A method for preparing a polymer compound, characterized in that, It comprises the following steps: (1) preparing raw materials: obtaining each raw material, the raw material includes: silane monomer, boron nitride, organic solvent, silanol, polyester resin, crosslinking catalyst, distilled water; (2) Preparation of boron nitride modified silicone resin: distilled water, boron nitride is added to the container containing silane monomer, stirring reaction at 200 230℃ for 3 5h, after the end of stirring reaction, cooling, distillation, adding organic solvent, stirring to obtain boron nitride modified silicone resin; (3) Preparation of modified polyester resin: the boron-nitrogen modified silicone resin prepared in step (2) and a cross-linking catalyst, a silanol, a polyester resin are mixed, and the mixture is continuously reacted at 110 130°C for 2 4h, and then an organic solvent is added, to obtain a modified polyester resin with a solid content of 62% 66%. During the preparation of boron-nitride modified silicone resin in step (2), the mixed solution in the container is collected at intervals 5h, the first hyperspectral image is taken as the initial stirring image, and all other hyperspectral images are taken as reaction images; the reflection feature intensity of each pixel in the initial stirring image is obtained according to the reflection feature significance of each pixel; the reflection feature intensity of all pixels in the initial stirring image is segmented by using a threshold segmentation algorithm to obtain a segmentation threshold; the pixel with a reflection feature intensity greater than the segmentation threshold is recorded as a feature pixel; the pixel at the position of the feature pixel in all reaction images is recorded as a matching pixel; the spectral similarity factor of each matching pixel in the reaction image is obtained according to the relationship between the feature pixel and the matching pixel; and the stirring time is controlled according to the spectral similarity factor distribution characteristics of each pixel.

2. The method for preparing a polymer compound according to claim 1, characterized in that, The silane monomer is at least one of methyl trimethoxysilane, dimethyl dimethoxysilane, phenyl trimethoxysilane, dimethyl trimethoxysilane, methyl triethoxysilane and dimethyl diethoxysilane; the boron nitride is amido dichloroborane or dimethylamine borane; the organic solvent is at least one of dimethylbenzene, butanol, toluene and propylene glycol methyl ether acetate; the crosslinking catalyst is titanium acid tetra-n-butyl ester or dibutyl tin dilaurate. The use amount of the silane monomer, the boron nitride, the distilled water and the organic solvent in the step (2) is 58-67% of the silane monomer, 3-10% of the boron nitride, 11-12% of the distilled water and 19-20% of the organic solvent in terms of mass percentage.

3. The method for preparing a polymer compound according to claim 1, characterized in that, The cooling in the step (2) is specifically cooling to 65-75 DEG C.

4. The method for preparing a polymer compound according to claim 1, characterized in that, The reflection characteristic intensity of each pixel in the initial stirring image obtained according to the reflection characteristic prominence degree of each pixel comprises:

5. The method for preparing a polymer compound according to claim 1, characterized in that, The mass ratio of the boron-nitride modified silicone resin, the silanol, the polyester resin, and the cross-linking catalyst in the step (3) is 1:(0.1 0.18):(0.2 0.55):(0.01 0.03).

6. The method of claim 1, wherein the polymer compound is prepared by the steps of: (a) dissolving the polymer compound in a solvent; (b) adding a non-solvent to the solution; and (c) precipitating the polymer compound. The reflection difference factor of each pixel is calculated, and the neighborhood difference sequence and the neighborhood characteristic difference sequence of each pixel are constructed, and the expression of the reflection characteristic intensity of each pixel in the initial stirring image is: The reflection difference factor of each pixel is calculated, and the neighborhood difference sequence and the neighborhood characteristic difference sequence of each pixel are constructed, and the expression of the reflection characteristic intensity of each pixel in the initial stirring image is: In the formula, is the reflection feature intensity of the i-th pixel in the initial stirring image, is the information entropy of the neighborhood feature difference sequence of the i-th pixel in the initial stirring image, is the total number of neighborhood paths in the pixel window of the i-th pixel in the initial stirring image, , respectively represent the neighborhood difference sequence of the x-th and y-th neighborhood path in the pixel window of the i-th pixel in the initial stirring image, represents the cosine similarity, and respectively represent the maximum reflection difference factor and the average reflection difference factor of all neighborhood pixels in the pixel window of the i-th pixel in the initial stirring image, is a natural constant, is a preset second adjustment parameter.

7. The method for preparing a polymer compound according to claim 6, characterized in that, For the initial stirring image, the maximum reflection band of each pixel is taken as the maximum reflection band of each pixel, the band with the highest occurrence frequency of the maximum reflection band of all pixels is taken as the significant reflection band, and the reflectivity of each pixel at the significant reflection band is taken as the significant reflectivity of each pixel; A pixel window is constructed with each pixel as the center, 8-neighbor directions of the center pixel in the pixel window are taken as each neighborhood path of the center pixel, all pixels on the neighborhood path are taken as neighborhood pixels, a square window is constructed with each neighborhood pixel as the center, and the significant reflectivity of all pixels in the square window is constructed into a reflection matrix of each neighborhood pixel according to the position of the pixel; The reflection matrix of each neighborhood pixel and the previous neighborhood pixel on the neighborhood path is taken as the input of the ANOSIM analysis algorithm, and the output is the global R value and the significance level value of each neighborhood pixel; The sum of the significance level value of each neighborhood pixel and a preset first adjustment parameter is calculated, the ratio of the global R value of each neighborhood pixel to the sum is calculated, the mean value of the significant reflectivity of all neighborhood pixels on the neighborhood path is calculated, the absolute value of the difference between the significant reflectivity of each neighborhood pixel and the mean value is calculated, and the product of the absolute value and the ratio is taken as the reflection difference factor of each neighborhood pixel. ​ 8. The method for preparing a polymer compound according to claim 1, characterized in that, The spectral similarity factor of each matching pixel in the reaction image is obtained according to the relationship between the feature pixel and the matching pixel, and the spectral similarity factor of each matching pixel in the reaction image is obtained according to the relationship between the feature pixel and the matching pixel, comprising: The Chameleon chameleon clustering algorithm is used to obtain the clustering cluster of each matching pixel in the initial stirring image and each reaction image; For each matching pixel in the reaction image at each collection time, the spectral vector angle between the matching pixel and the feature pixel at the corresponding position is calculated, which is denoted as the first spectral vector angle, the spectral vector angle between the matching pixel and the matching pixel at the corresponding position in the reaction image at the previous collection time is calculated, which is denoted as the second spectral vector angle, and the sum of the first spectral vector angle and the second spectral vector angle is calculated, which is denoted as the first sum value; The difference absolute value between the average significant reflectivity of the corresponding feature pixel of each matching pixel in the clustering cluster of the initial stirring image and the average significant reflectivity of all pixels in the clustering cluster of each matching pixel in the reaction image is calculated, which is denoted as the first difference absolute value, the difference absolute value between the average significant reflectivity of all pixels in the clustering cluster of each matching pixel in the reaction image and the average significant reflectivity of all pixels in the clustering cluster of the corresponding matching pixel in the reaction image at the previous collection time is calculated, which is denoted as the second difference absolute value, and the sum of the first difference absolute value and the second difference absolute value is calculated, which is denoted as the second sum value, and the ratio of the first sum value to the second sum value is taken as the spectral similarity factor of each matching pixel in the reaction image.

9. The method of claim 1, wherein the polymer compound is prepared by the steps of: (a) dissolving the polymer compound in a solvent; (b) adding a non-solvent to the solution; and (c) precipitating the polymer compound. The control stirring time comprises: A preset adjustment interval, the spectral similarity factors of each matching pixel in the adjustment interval at all collection times are sorted in time sequence as the spectral similarity sequence of each matching pixel, the spectral similarity sequences of all matching pixels in the adjustment interval are arranged in rows to construct a spectral similarity matrix, and the trend item of each element in each spectral similarity sequence in each adjustment interval is obtained by using the STL sequence decomposition algorithm; The expression of the reaction change persistence factor of each matching pixel in each adjustment interval is: In the formula, represents the reaction change persistence factor of the fth matching pixel in the zth adjustment interval, and respectively represent the maximum spectral similarity factor, the minimum spectral similarity factor and the mean of all spectral similarity factors in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval; is the total number of elements in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, is the trend item intensity of the mth element in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval. The expression of the stirring reaction stability characteristic coefficient of each adjustment interval is: In the formula, is the stirring reaction stability characteristic coefficient of the zth adjustment interval, is the total number of matching pixels, is the information entropy of all elements in the spectral similarity sequence of the fth matching pixel in the zth adjustment interval, respectively represent the spectral similarity matrix of the zth and the z-1th adjustment interval, is the Euclidean distance, and norm is a normalization function. A stirring time threshold is preset, if the stirring reaction stability characteristic coefficient of the adjustment interval is less than the stirring time threshold, the stirring reaction time of one adjustment interval is increased, otherwise, the stirring reaction is stopped.

10. A high molecular compound production system comprising a storage, a processor, and a computer program stored in the storage and run on the processor, characterized by, The processor executes the computer program to realize the steps of the method of any one of claims 1-9. The processor executes the computer program to realize the steps of the method of any one of claims 1-9.

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