High-molecular compound preparation method and system

Abstract

The invention relates to the technical field of high-molecular compound preparation, in particular to a high-molecular compound preparation method and system.The method comprises the steps that distilled water and boron nitride are added into a container containing silane monomers, stirring reaction is conducted for 3-5 h, and a hyperspectral image of a mixed solution in the container in the stirring reaction process is collected; the method comprises the following steps: acquiring spectral similarity factors of matched pixels in a hyperspectral image, judging the fullness degree of a stirring reaction according to the distribution characteristics of the spectral similarity factors of the pixels, completing the stirring reaction, mixing the prepared boron nitride modified organic silicon resin, silanol, polyester resin and a crosslinking catalyst, continuously reacting for 2-4 hours at 110-130 DEG C, adding an organic solvent, and uniformly stirring to obtain the boron nitride modified organic silicon resin. The solid content of the modified polyester resin is 62-66%. The invention aims to improve the performance and prolong the service life of the prepared modified polyester resin, and realizes the preparation method of the high-molecular compound.

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 a 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 an 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: In a first aspect, the present application provides a high molecular compound preparation method, which comprises the following steps: (1) preparing raw materials: obtaining various raw materials, including silane monomer, boron nitride, organic solvent, silanol, polyester resin, cross-linking catalyst and distilled water; (2) preparing boron nitride modified organic silicon resin: adding distilled water and boron nitride to a container containing silane monomer, and stirring at 200 230℃ for 3 5h, then cooling, distilling, adding organic solvent and stirring to obtain boron nitride modified organic silicon resin; (3) preparing modified polyester resin: mixing the boron nitride modified organic silicon resin prepared in step (2), cross-linking catalyst, silanol and polyester resin, and stirring at 110 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; 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.

[0005] Preferably, the silane monomer is: 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.

[0006] 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.

[0007] Preferably, step (2) cooling specifically involves cooling to 65°C~75°C.

[0008] 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).

[0009] Preferably, obtaining the reflection feature intensity of each pixel in the initial stirring image based on the saliency of the reflection features of each pixel includes: Calculate the reflectance difference factor of each pixel's neighboring pixels, and construct the neighborhood difference sequence and the neighborhood feature difference sequence of each pixel. The expression for the reflectance feature intensity of each pixel in the initial stirring image is: wherein, 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.

[0010] Preferably, the reflection difference factor of each neighborhood pixel of each pixel is calculated, and the neighborhood difference sequence and the neighborhood feature difference sequence of each pixel are constructed, comprising: 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 frequency of occurrence 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, the 8-neighborhood direction of the center pixel in the pixel window is 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 taken to construct the 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 value 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 value 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 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 of the neighborhood pixels from the center pixel, as the neighborhood difference sequence of each neighborhood path. The reflectance difference factors of the neighborhood pixels on all neighborhood paths in the pixel window of each pixel are sorted in order from large to small, as the neighborhood feature difference sequence of each pixel.

[0011] 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 of each matching pixel in the reaction image is obtained according to the relationship between the feature pixel and the matching pixel, including: The Chameleon chameleon clustering algorithm is used to obtain each clustering cluster of all feature pixels in the initial stirring image and all matching pixels in each reaction image. 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 value of the first spectral vector angle and the second spectral vector angle is calculated, denoted as the first sum value. The absolute value of the difference between the mean value of the significant reflectivity of the corresponding feature pixel of each matching pixel in the clustering cluster to which the initial stirring image belongs and the mean value of the significant reflectivity of all pixels in the clustering cluster to which each matching pixel in the reaction image belongs is calculated, denoted as the first absolute difference value, the absolute value of the difference between the mean value of the significant reflectivity of all pixels in the clustering cluster to which each matching pixel in the reaction image belongs and the mean value of the significant reflectivity of all pixels in the clustering cluster to which the matching pixel at the corresponding position in the reaction image at the previous acquisition time belongs is calculated, denoted as the second absolute difference value, and the sum value of the first absolute difference value and the second absolute difference value is calculated, denoted as the second sum value. 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.

[0012] Preferably, the control stirring time comprises: A preset adjustment interval is set, the spectral similarity factors of each matching pixel in the adjustment interval at all acquisition 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 items of the elements in each spectral similarity sequence in each adjustment interval are obtained by using the STL sequence decomposition algorithm. The expression for the duration factor of response change for each matched pixel in each adjustment interval is: In the formula, This represents the duration factor of the response change of the f-th matching pixel in the z-th adjustment interval. as well as Let 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 f-th matching pixel in the z-th adjustment interval, respectively. Let f be the total number of elements in the spectral similarity sequence of the f-th matching pixel in the z-th adjustment interval. Let m be the trend term intensity of the m-th element in the spectral similarity sequence of the f-th matching pixel in the z-th adjustment interval; The expression for the stability characteristic coefficient of the stirred reaction in each adjustment interval is as follows: In the formula, Let be the characteristic coefficient of the stirring reaction stability in the z-th adjustment interval. To match the total number of pixels, Let be the information entropy of all elements within the spectral similarity sequence of the f-th matching pixel in the z-th adjustment interval. Let these represent the spectral similarity matrices of the z-th and z-1-th adjustment intervals, respectively. Here, Euclidean distance is used, and norm is the normalization function. A preset stirring time threshold is set. If the stability characteristic coefficient of the stirring reaction in the adjustment interval is less than the stirring time threshold, the stirring reaction time of the adjustment interval is increased by one interval; otherwise, the stirring reaction is stopped.

[0013] Secondly, embodiments of the present invention also provide a polymer compound preparation system, including a memory, a processor, and a computer program stored in the memory and running on the processor, wherein the processor executes the computer program to implement the steps of any of the methods described above.

[0014] The present invention has at least the following beneficial effects: The application obtains the reflection feature intensity of each image element by the initial stirring image reflectivity difference feature, identifies the feature image element and the matching image element according to the reflection feature intensity, avoids the analysis on all image elements in the stirring solution hyperspectral image, determines the image element with significant reflectivity change feature in the neighborhood range on the basis of saving the computing resource, and can more accurately evaluate the fullness of the stirring reaction. The spectral similarity factor is constructed between the feature image element and the matching image element, 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 image elements in the adjustment interval, the change persistence of the spectral feature similarity degree of all matching image elements in the adjustment interval and the reaction stability feature 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 property is prepared, and the alkali resistance of the modified polyester resin is improved. BRIEF DESCRIPTION OF DRAWINGS

[0015] 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 only show some embodiments of the present application, and for those skilled in the art, other drawings can be obtained without creative labor.

[0016] 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. Figure 2 An adjustment stirring reaction time flow chart is shown in the figure. Figure 3 A modified polyester resin preparation flow chart is shown in the figure. Figure 4 An initial stirring image Chameleon chameleon clustering result figure is shown in the figure. DETAILED DESCRIPTION

[0017] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined application purpose, the specific implementation, structure, features and effects of the high polymer compound preparation method and system according to the present application are described in detail as follows by combining the drawings and the 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.

[0018] 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.

[0019] The application provides a high polymer compound preparation method and system.

[0020] Preparation of the polyester resin: Ternary alcohol: 134 g of trimethylolpropane; binary alcohol: 10.4 g of neopentyl glycol; isophthalic acid: 107.9 g; dimethylbenzene: 6.7 g; organic solvent: 200 g of propylene glycol methyl ether acetate.

[0021] The 134 g of trimethylolpropane and the 10.4 g of neopentyl glycol were uniformly mixed and heated to 80 °C, and then the 107.9 g of isophthalic acid and the 6.7 g of dimethylbenzene were added; after heating at 200 °C for 2 h, the temperature was raised to 230 °C, heated for 2 h, and then the temperature was lowered to 90 °C, and the 200 g of propylene glycol methyl ether acetate was added to obtain the polyester resin in each example.

[0022] Example 1 Please refer to Figure 1 which shows a step flow chart of a high polymer compound preparation method provided by the example, and the method comprises the following steps: Step S001, obtaining the preparation raw materials of the modified polyester resin.

[0023] (1) Preparation of raw materials Silane monomer: methyltrimethoxysilane, dimethyldimethoxysilane, and phenyltrimethoxysilane; Boron nitride: amido dichloroborane; organic solvent: dimethylbenzene and propylene glycol methyl ether acetate; Silanol: KR220L solid silanol, weight average molecular weight: 850, and hydroxyl content: 3% 5 w%; Polyester resin: polyester resin obtained by the synthesis example; crosslinking catalyst (tetra-n-butyl titanate); distilled water.

[0024] (2) Preparation of boron nitride modified silicone resin 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 amido dichloroborane were slowly added to the four-necked flask, and the stirrer was started to stir at 200 °C for 3 h. 5h. Distillation was performed after cooling to 75°C to distill off low-boiling small molecules, and then 2.3 g of the organic solvent xylene was poured into the four-necked flask. After mixing and stirring, an emulsion was obtained, and a boron-nitrogen modified silicone resin was obtained.

[0025] (3) Preparation of modified polyester resin After mixing 70 g of the polyester resin obtained in the synthesis example, 23 g of silanol, 230 g of the boron-nitrogen modified silicone resin, and 2.3 g of tetra-n-butyl titanate, 50 g of propylene glycol methyl ether acetate was added after continuous reaction at 110°C for 2 h, heating and stirring were stopped, and the product was discharged after cooling, thereby obtaining a modified polyester resin having a solid content of 62%.

[0026] Example 2 (1) Preparation of raw materials Silane monomer: dimethyltrimethoxysilane, phenyltrimethoxysilane; Boron-nitrogen compound: aminodichloroborane; organic solvent: toluene, propylene glycol methyl ether acetate; Silanol: KR220L solid silanol having a weight average molecular weight of 850 and a hydroxyl group content of 3% 5w%; Polyester resin: polyester resin obtained in the synthesis example; crosslinking catalyst (dibutyltin dilaurate); distilled water.

[0027] (2) Preparation of boron-nitrogen modified silicone resin The silane monomers, 6 g of dimethyltrimethoxysilane 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. 1.61 g of distilled water and 0.8 g of aminodichloroborane were slowly added to the four-necked flask, and the stirrer was turned on. The mixture was 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.

[0028] (3) Preparation of modified polyester resin After mixing 92 g of the polyester resin obtained in the synthesis example, 34 g of silanol, 230 g of the boron-nitrogen modified silicone resin, and 3 g of dibutyltin dilaurate, 40 g of propylene glycol methyl ether acetate was added after continuous reaction at 120°C for 3 h, heating and stirring were stopped, and the product was discharged after cooling, thereby obtaining a modified polyester resin having a solid content of 64%.

[0029] Example 3 (1) Preparation of raw materials Silane monomer: methyltriethoxysilane, dimethyldiethoxysilane; Borazene: aminodichloroborane; organic solvent: butanol, propylene glycol methyl ether acetate; Silanol: KR220L solid silanol, weight average molecular weight 850, hydroxyl content 3% 5w%; Polyester resin: polyester resin obtained in the synthetic example; crosslinking catalyst (tetra-n-butyl titanate); distilled water.

[0030] (2) Preparation of borazene-modified silicone resin Mixing 3.56 g of methyl triethoxysilane and 2.96 g of dimethyldiethoxysilane, pouring into a four-necked flask equipped with a condenser, a stirrer, a thermometer, and an addition funnel, slowly adding 1.22 g of distilled water and 1.1 g of dimethylamine borane into the four-necked flask, starting the stirrer, and stirring at 210°C for 3 h 5h. After cooling to 70°C, distillation is performed to remove low-boiling small molecules, then 2.1 g of organic solvent butanol is poured into the four-necked flask, and after uniform mixing and stirring, an emulsion is obtained, and a borazene-modified silicone resin is obtained.

[0031] (3) Preparation of modified polyester resin Mixing 120 g of polyester resin obtained in the synthetic example, 40 g of silanol, 230 g of borazene-modified silicone resin, and 6 g of tetra-n-butyl titanate, and continuously reacting at 120°C for 3 h, then adding 30 g of propylene glycol methyl ether acetate and 20 g of butanol, stopping heating and stirring, and cooling and discharging, a modified polyester resin with a solid content of 66% is obtained.

[0032] The mixed solution in the stirring reaction process during the preparation of the borazene-modified silicone resin in each example is imaged by a hyperspectral imager, and the imaging starts at the beginning of the stirring reaction, with an imaging time interval of 1 min. The imaging time interval can be set by the implementer according to the actual situation, and the present example does not limit this. The hyperspectral image is collected at a top view angle. In order to avoid the loss of image details due to the presence of much noise in the stirring solution hyperspectral image, the obtained hyperspectral image needs to be preprocessed. The stirring solution hyperspectral image is denoised using a mean filtering algorithm. The mean filtering algorithm is a known technology, and the present example does not go into detail. The implementer can choose other algorithms to denoise the stirring solution hyperspectral image according to the actual situation.

[0033] At this point, the time-series-based stirring solution hyperspectral image can be obtained. The first stirring solution hyperspectral image collected is denoted as the initial stirring image, and all subsequent stirring solution hyperspectral images collected are denoted as reaction images.

[0034] In step S002, the reflectance feature intensity of each pixel is obtained by the initial stirring image reflectance difference feature, the feature pixel and the matching pixel are determined according to the reflectance feature intensity, the spectral similarity factor is constructed according to the spectral feature of the feature pixel and the matching pixel, 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 the matching pixels in the adjustment interval, and the stirring reaction time is adjusted.

[0035] Specifically, first, the silane monomer is poured into the container, distilled water and boron nitride are added, and the stirring reaction is carried out 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 according to the spectral similarity factor distribution characteristics of each pixel, the stirring reaction is completed, and the prepared boron nitride modified organic silicone resin, silanol, polyester resin and crosslinking catalyst are mixed in the container. At 110 130℃, the reaction is continued for 2-4h, and then an organic solvent is added to obtain a modified polyester resin with a solid content of 62% Figure 2 66%. The stirring reaction time length adjustment process is shown in the figure Figure 3 The stirring reaction stability characteristic coefficient of each adjustment interval is constructed as follows: In the initial stirring image, the greater the difference between the reflectance of the pixel and the surrounding environment, the more the spectral feature change condition of the pixel can be used to measure the degree of completion of the stirring reaction 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 means 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 complete. Now the initial stirring image is analyzed.

[0036] The maximum wavelength of the reflectance of each pixel in the initial stirring image is taken as the maximum reflection wavelength of each pixel, the wavelength with the highest frequency among the maximum reflection wavelengths of all pixels in the initial stirring image is taken as the significant reflection wavelength of the initial stirring image, and the reflectance of each pixel in the significant reflection wavelength of the initial stirring image is taken as the significant reflectance of each pixel, denoted as a.

[0037] 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 recorded as the neighborhood paths of the center pixel, the pixels on all neighborhood paths in the pixel window are recorded as the 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.

[0038] 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, the global R value and the significance level value p are given to the jth pixel on the neighborhood path, wherein the greater the global R value, the greater 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 will not be described in detail in this embodiment.

[0039] Based on the above analysis, a reflection difference factor is constructed to represent the significant degree of the reflection characteristics of each pixel in the initial stirring image, and the expression is: 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, is the global R value of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, is the significance level value p of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, is the significant reflectivity of the jth neighborhood pixel on the xth neighborhood path of the ith pixel in the initial stirring image, is the average value of the significant reflectivity of all neighborhood pixels on the xth neighborhood path of the ith pixel in the initial stirring image; is a preset first adjustment parameter to prevent the denominator from being 0, in this embodiment , the implementer can set it according to the actual situation, and this embodiment does not limit it.

[0040] 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 greater, that is The greater the difference between the significant reflectivity of the neighborhood pixel and the average significant reflectivity of all neighborhood pixels on the neighborhood path where the neighborhood pixel is located, the greater the reflectance difference factor The greater the difference between the significant reflectivity of the neighborhood pixel and the average significant reflectivity of all neighborhood pixels on the neighborhood path where the neighborhood pixel is located, the greater the reflectance difference factor The greater the difference between the significant reflectivity of the neighborhood pixel and the average significant reflectivity of all neighborhood pixels on the neighborhood path where the neighborhood pixel is located, the greater the reflectance difference factor

[0041] The greater the difference between the significant reflectivity of the neighborhood pixel and the average significant reflectivity of all neighborhood pixels on the neighborhood path where the neighborhood pixel is located, the greater the reflectance difference factor The greater the difference between the significant reflectivity of the neighborhood pixel and the average significant reflectivity of all neighborhood pixels on the neighborhood path where the neighborhood pixel is located, the greater the reflectance difference factor In the formula, H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and

[0042] H (i) is the reflectance feature intensity of the i-th pixel in the initial stirring image, and The greater, the greater the fluctuation of the reflection difference factor of each neighborhood pixel in the neighborhood range of the pixel; meanwhile, the smaller the sum of the cosine similarity between the neighborhood difference sequences corresponding to all neighborhood paths in the i-th pixel window in the initial stirring image, that is The smaller, the less similar the reflection difference conditions of the neighborhood pixels on each neighborhood path in the pixel window; meanwhile, the greater the difference between the maximum reflection difference factor and the average reflection difference factor of all neighborhood pixels in the pixel window, that is The greater, the greater the difference between the maximum reflection difference condition and the average reflection difference condition in the neighborhood range of the pixel, the more significant the reflectance difference feature in the neighborhood range of the pixel at the corresponding position of the pixel, and the more the pixel should be used as a feature pixel for subsequent analysis, that is, the reflection feature strength The greater.

[0043] All the reflection feature strengths of the pixels in the initial stirring image are arranged in ascending order to construct a reflection feature strength sequence, the reflection feature strength sequence is taken as input, and the OTSU thresholding method is used to obtain a segmentation threshold of the reflection feature strength sequence. The pixels with a reflection feature strength greater than the segmentation threshold are recorded as feature pixels . The pixels at the positions of the feature pixels in all the reaction images are recorded as matching pixels All the feature pixels in the initial stirring image are taken as nodes of an undirected graph, the absolute value of the difference between the reflection feature strengths of the nodes is taken as a distance measurement method, and the 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 acquisition time is taken as a node of an undirected graph, the absolute value of the difference between the reflection feature strengths of the nodes is taken as a distance measurement method, and the Chameleon clustering algorithm is used to obtain each clustering cluster in the reaction image at each acquisition time, denoted as g. The Chameleon clustering algorithm is a known technology, and will not be described in detail in this embodiment. The Chameleon clustering result of the initial stirring image is shown in Figure 4 .

[0044] 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: In the formula, is the spectral similarity factor of the f-th matching pixel in the reaction image at the t-th acquisition time, is the f-th matching pixel in the reaction image at the t-th acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth feature pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, is the spectral vector angle between the fth matching pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time; is the average of the apparent reflectance of all pixels in the cluster to which the fth feature pixel in the initial stirring image belongs, is the average of the apparent reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the tth acquisition time belongs, is the average of the apparent reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the tth acquisition time belongs.

[0045] When the sum of the spectral vector angle between the fth feature pixel in the initial stirring image and the fth matching pixel in the reaction image at the tth acquisition time, and the spectral vector angle between the fth matching pixel in the reaction image at the tth acquisition time and the fth matching pixel in the reaction image at the t-1th acquisition time is smaller, that is, is smaller, it indicates that the matching degree of the spectral features between the pixels is higher; at the same time, when the sum of the absolute value of the difference between the average of the apparent reflectance of all pixels in the cluster to which the fth feature pixel in the initial stirring image belongs and the average of the apparent reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the tth acquisition time belongs, and the absolute value of the difference between the average of the apparent reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the tth acquisition time belongs and the average of the apparent reflectance of all pixels in the cluster to which the fth matching pixel in the reaction image at the t-1th acquisition time belongs is smaller, that is, is smaller, it indicates that the difference of the apparent reflectance between the clusters to which the pixels correspond is smaller, and the spectral features of the pixels at the corresponding positions at the tth acquisition time are more similar to those at the corresponding positions in the initial stirring image and the reaction image at the t-1th acquisition time, and the spectral similarity factor is larger.

[0046] Each 30 min is recorded as an adjustment interval, and the zth adjustment interval is taken as an example. The spectral similarity sequence of the pixels is constructed according to the spectral similarity factors of each matching pixel in the zth adjustment interval at all acquisition times in chronological order, and is recorded as H. The spectral similarity sequence of all matching pixels in the adjustment interval is respectively taken as a row to construct the spectral similarity matrix of the adjustment interval, and is recorded 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), and is recorded as Since the STL sequence decomposition algorithm is a known technology, this embodiment will not be described in detail.

[0047] Based on the above analysis, the stirring reaction characteristic stability coefficient is constructed to represent the adjustment interval of the stirring reaction, and the expression is: 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 average 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, and in the embodiment , the implementer can set it according to the actual situation, and the embodiment does not limit it; 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, represents the spectral similarity matrix of the zth adjustment interval, represents the spectral similarity matrix of the z-1th adjustment interval, is the Euclidean distance between the matrix and , and norm is a normalization function, so that the value range of is in the range of [0, 1].

[0048] 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 greater, that is, is greater, it indicates that the spectral similarity factor of the matching pixel in the adjustment interval changes more, and the stirring reaction in the adjustment interval is more sufficient; at the same time, when the average of all spectral similarity factors in the spectral similarity sequence is smaller, that is, is smaller, 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 greater, that is, The greater, the more obvious the change of the spectral similarity factor of the matching pixels in the adjustment interval, the more significant the change of the stirring reaction at the corresponding position of the matching pixels, and the reaction change persistence factor The greater.

[0049] When the sum of the reaction change persistence factor of all matching pixels in the zth adjustment interval and the product of the information entropy of the spectral similarity sequence of all matching pixels in the adjustment interval is greater, that is, The greater, the more significant the change of the spectral similarity factor of all matching pixels in the adjustment interval, the more likely the stirring reaction at the corresponding position of all matching pixels in the adjustment interval is still in progress, and the stirring reaction time should be extended at this time to make the stirring reaction proceed fully; at the same time, when the Euclidean distance of the spectral similarity matrix between 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 at the corresponding position of all matching pixels in the zth adjustment interval, and the stirring reaction time should be extended at this time to make the stirring reaction proceed fully, that is, the stirring reaction stability characteristic coefficient The greater.

[0050] At this point, the stirring reaction stability characteristic coefficient of each adjustment interval can be obtained, and the stirring time threshold value In the present embodiment , the implementer can set it according to the actual situation, and the present 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 an adjustment interval is increased, that is, the stirring time is extended by 30 min; on the contrary, 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.

[0051] At this point, the optimal stirring reaction time of each embodiment can be obtained by the above-mentioned method, 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.

[0052] Step S003: preparing a modified polyester resin according to the obtained boron nitride modified silicone resin with sufficient stirring reaction, and testing the performance of the modified polyester resin.

[0053] The performance of the obtained modified polyester resin is tested as follows: Thermogravimetric analysis: tested by a thermogravimetric analyzer, under a high-purity nitrogen atmosphere, with a heating rate of 10 ℃ / min.

[0054] Heat resistance performance analysis: the treated test piece is coated with polyester modified resin, and after baking at 280℃ for 10min, it is put into a potential difference meter checked constant temperature oven, and the temperature is increased at 5℃ / min. When the furnace temperature reaches the required temperature, the timing starts. After the sample is subjected to continuous high temperature, it is taken out and cooled to room temperature (25℃). The surface condition of the coating is observed with a magnifying glass. If there is no cracking or peeling phenomenon, it means that the heat resistance of the coating is good.

[0055] Adhesion test: test according to GB / T9286-1998.

[0056] Paint film impact strength test: test according to GB / T1732-93.

[0057] Paint film flexibility test: test according to GB / T1731-39.

[0058] The performance test results of the modified polyester resin are shown in Table 1.

[0059] Table 1 Performance test table So far, a high polymer compound preparation method and system can be realized according to the above method.

[0060] Based on the same inventive concept as the above method, the present application also provides 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. When the processor executes the computer program, the steps of any one of the above high polymer compound preparation methods are realized.

[0061] In summary, the present application comprehensively considers the change duration and reaction stability characteristics of the spectral similarity degree of all matching image elements in the adjustment interval, which can more accurately measure the sufficient condition of the stirring reaction in the adjustment interval, and use it as the basis for adjusting the stirring reaction time. The stirring reaction time can be adjusted according to the characteristics of the stirring solution in the adjustment interval, and then a boron nitride modified organic silicon resin with good performance is obtained, and finally a modified polyester resin with good heat resistance and mechanical properties is obtained.

[0062] It should be noted that: the above-mentioned sequence of the embodiments of the present application is only for description, not representing the advantages and disadvantages of the embodiments. The above describes 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, multitasking and parallel processing are possible or may be advantageous.

[0063] The various embodiments in the specification are described in progressive manner, and the same or similar parts between the various embodiments can be mutually referred to, and each embodiment focuses on the difference from other embodiments.

[0064] The above description is merely preferred embodiments of the present application, and is not intended to 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 wavelength of each pixel is taken as the maximum reflection wavelength of each pixel, the wavelength with the highest frequency of the maximum reflection wavelength of all pixels is taken as the significant reflection wavelength, and the reflectivity of each pixel at the significant reflection wavelength is taken as the significant reflectivity of each pixel; The 8-neighborhood direction of the center pixel in the pixel window is taken as each neighborhood path of the center pixel, all pixels on the neighborhood path are taken as neighborhood pixels, and a square window is constructed with each neighborhood pixel as the center. 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 value 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 value 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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