Preparation method of organic polymeric flocculant for water treatment

Abstract

The invention relates to the technical field of preparation of flocculants, in particular to a preparation method of an organic polymeric flocculant for water treatment, which comprises the following steps: adding acrylic acid and tetramethylguanidine into a reactor, heating and stirring to obtain a tetramethylguanidine acrylate solution; the preparation method comprises the following steps: fully dissolving sorbitan monooleate in a cyclohexane solution under a nitrogen condition, then adding acrylamide, vinyl guanamine and a synergist, and heating and stirring to obtain a mixture solution; and mixing the tetramethylguanidine acrylate solution with the mixture solution, then adding an initiator, stirring for polymerization reaction, and controlling and adjusting the reaction temperature in the polymerization reaction process to finally obtain the organic polymeric flocculant. The invention aims to avoid the adverse effect on the polymerization reaction caused by too high or too low reaction temperature, thereby ensuring the effectiveness of the polymerization reaction and the intrinsic viscosity of the flocculant after the polymerization reaction.

Description

Technical Field

[0001] This application relates to the field of flocculant preparation technology, specifically to a method for preparing an organic polymeric flocculant for water treatment. Background Technology

[0002] Organic polymeric flocculants, as important water treatment agents, play a crucial role in solid-liquid separation during wastewater treatment and production processes. Most existing processes prepare organic polymeric flocculants by adding initiators and employing polymerization reactions. However, during the polymerization process, if the reaction temperature is too low, the initiator decomposes slowly, resulting in low activity of the reactants and affecting the formation of polymerization products. Conversely, if the reaction temperature is too high, the polymerization rate accelerates, causing the reaction to terminate rapidly and ultimately affecting the intrinsic viscosity of the polymerization products.

[0003] Therefore, in order to ensure the effectiveness of the polymerization reaction and the intrinsic viscosity of the flocculant after polymerization, it is necessary to accurately control and adjust the reaction temperature during the polymerization process to reduce the influence of the reaction temperature on the intrinsic viscosity of the flocculant after polymerization.

[0004] In the process of preparing organic polymer flocculants through polymerization, most existing technologies carry out polymerization reactions at a preset fixed reaction temperature. However, due to the exothermic phenomenon in the polymerization process, local heat accumulation is easily generated in the polymerization reaction solution. Existing technologies cannot fully consider the characteristics of local heat accumulation to accurately control and adjust the reaction temperature, making the actual reaction temperature unsuitable for the polymerization process. This results in the problem of poor intrinsic viscosity of the organic polymer flocculant after polymerization. Summary of the Invention

[0005] To address the aforementioned technical problems, this application provides a method for preparing an organic polymeric flocculant for water treatment, thereby resolving the existing issues.

[0006] The present application discloses a method for preparing an organic polymeric flocculant for water treatment, which adopts the following technical solution: One embodiment of this application provides a method for preparing an organic polymeric flocculant for water treatment, the method comprising the following steps: S1, by weight, 11-14 parts of acrylic acid and 19-27 parts of tetramethylguanidine are added to a reactor and heated and stirred to obtain a tetramethylguanidine acrylate solution; S2, under nitrogen conditions, 2-4 parts of sorbitan monooleate are fully dissolved in 50-100 parts of cyclohexane solution, followed by the addition of 23-27 parts of acrylamide, 0.5-1 parts of vinylguanidine, and 5-12 parts of synergist, and the mixture is heated and stirred to obtain a mixed solution. S3, mix tetramethylguanidine acrylate solution and mixture solution, then add initiator and stir to carry out polymerization reaction. By controlling and adjusting the reaction temperature during the polymerization process, the organic polymer flocculant is finally obtained; The control and adjustment method is as follows: S301, collects absorption spectrum data of the polymerization reaction solution and reaction temperature data during the polymerization reaction process; S302, analyze the correlation between the reaction temperature and polymerization intensity characteristic values ​​at each sampling point in the polymerization reaction solution during each local sampling period, as well as the reaction temperature differences between sampling points, and determine the cumulative heat influence at each sampling point at each sampling time. S303. Based on the differences in the cumulative heat influence between all sampling points at each sampling time and the distance between the sampling points, and combined with the maximum value of the cumulative heat influence of all sampling points at each sampling time, the reliability of thermal imbalance at each sampling time is determined. S304. Based on the difference between the thermal imbalance confidence level and its segmentation threshold, and the actual reaction temperature obtained from the average reaction temperature at all sampling points, the expected reaction temperature at the current sampling moment is obtained. The PID controller is used to control and adjust the reaction temperature during the polymerization process based on the temperature error between the expected reaction temperature and the actual reaction temperature.

[0007] Preferably, in step S1, the heating temperature is 45-60°C, and the stirring time is 3-5 hours to carry out the neutralization reaction. After the neutralization reaction is completed, a tetramethylguanidine acrylate solution is obtained.

[0008] Preferably, the temperature for heating in step S2 is 45-60°C.

[0009] Preferably, the initiator added in step S3 is 1-5 parts by weight.

[0010] Preferably, the method for obtaining the polymerization strength characteristic value is as follows: Calculate the difference between the absorbance vectors at each acquisition point location and the previous acquisition time; Calculate the time difference between each acquisition time and the previous acquisition time, and record the ratio of the difference to the time difference as the aggregation intensity characteristic value of each acquisition position at each acquisition time.

[0011] Preferably, the method for determining the reliability of the thermal imbalance is as follows: The significance of the heat accumulation difference at each collection time is determined based on the differences in the heat accumulation influence between all collection points at each collection time and the distance between the locations. The exponentially normalized result of the product of the significance of the difference in heat accumulation at each collection time and the maximum value of the influence of heat accumulation at all collection points at each collection time is denoted as the characteristic value of the heat imbalance of the polymerization system at each collection time during the polymerization process. The thermal imbalance feature vector at the current acquisition time is a vector composed of the thermal imbalance feature values ​​of all acquisition times within the preset time period before the current acquisition time in chronological order. The first-order difference vector of the thermal imbalance feature vector is then calculated. The ratio of the number of all positive elements in the first-order difference vector to the total number of elements. ; Calculate the mean of all positive elements in the first-order difference vector. ; ratio with the mean The product of the two values ​​is denoted as the credibility weight at the current acquisition time. The exponentially normalized result of the product of the credibility weight at the current acquisition time and the thermal imbalance characteristic value at the current acquisition time is denoted as the thermal imbalance credibility at the current acquisition time.

[0012] Preferably, the method for determining the significance of the heat accumulation difference at each acquisition time is as follows: The cumulative heat influence of all sampling points at each sampling time is arranged into a sequence in ascending order; For any two adjacent elements in the sequence, calculate the numerical difference between the next adjacent element and the previous element; calculate the Euclidean distance between the corresponding sampling point positions of the next adjacent element and the previous element; calculate the ratio of the numerical difference to the Euclidean distance. The sum of the ratios calculated between all adjacent elements in the sequence is used as the significance of the cumulative thermal difference at each acquisition time.

[0013] Preferably, the method for obtaining the desired reaction temperature at the current sampling time is as follows: The average reaction temperature at all sampling points at the current sampling time is recorded as the actual reaction temperature at the current sampling time. In the formula, This represents the desired reaction temperature at the current sampling moment during the polymerization process. This represents the actual reaction temperature at the current sampling moment. To assess the reliability of the thermal imbalance at the current sampling moment during the polymerization reaction. The threshold for determining the reliability of thermal imbalance during the historical process of the polymerization reaction; the historical process consists of all acquisition times prior to the current acquisition time.

[0014] Preferably, the method for obtaining the segmentation threshold is as follows: inputting the thermal imbalance confidence level at all collection moments in the historical process into the maximum inter-class variance algorithm, and using the maximum inter-class variance algorithm to obtain the segmentation threshold of the thermal imbalance confidence level.

[0015] Preferably, the step of using a PID controller to control and adjust the reaction temperature during the polymerization process based on the temperature error between the desired reaction temperature and the actual reaction temperature includes: The actual reaction temperature and the desired reaction temperature at the current acquisition moment during the polymerization process are transmitted to the PID controller. The PID controller inputs the control signal for the reaction temperature based on the temperature error between the actual reaction temperature and the desired reaction temperature, and transmits the control signal for the reaction temperature to the heating device. The heating device controls the actual reaction temperature during the polymerization process to approach the desired reaction temperature.

[0016] This application has at least the following beneficial effects: (1) This invention considers the influence of heat accumulation in the polymerization reaction solution on the polymerization reaction intensity, and accurately measures the influence of heat accumulation at different collection points in the polymerization reaction solution, which is beneficial to fully consider the characteristics of local heat accumulation and accurately control and adjust the reaction temperature.

[0017] (2) By analyzing the significant difference in heat accumulation between different sampling points in the polymerization reaction solution and combining the characteristics of the influence of heat accumulation, the present invention measures the characteristic value of heat imbalance in the polymerization reaction system, which more clearly reflects the real-time heat distribution characteristics in the polymerization reaction process, and is conducive to the accurate control and adjustment of the reaction temperature in the polymerization reaction system in the future.

[0018] (3) This invention analyzes the continuous upward trend of thermal imbalance characteristics during the polymerization reaction, sets a confidence weight, and thus accurately measures the confidence level of the thermal imbalance state during the polymerization reaction. It also considers the difference between the confidence level of thermal imbalance and the threshold of imbalance confidence in the historical process, adjusts the actual reaction temperature, avoids the adverse effects of excessively high or low reaction temperature on the polymerization reaction, and thus ensures the effectiveness of the polymerization reaction and the characteristic viscosity of the flocculant after the polymerization reaction. Attached Figure Description

[0019] To more clearly illustrate the technical solutions and advantages in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1A flowchart of a method for preparing an organic polymeric flocculant for water treatment provided in this application; Figure 2 This is a flowchart illustrating the method for controlling and adjusting the reaction temperature during the polymerization process provided in this application. Detailed Implementation

[0021] To further illustrate the technical means and effects adopted by this application to achieve the intended purpose of the invention, the following, in conjunction with the accompanying drawings and preferred embodiments, details the specific implementation, structure, features, and effects of a method for preparing an organic polymer flocculant for water treatment according to this application. In the following description, different "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable form.

[0022] 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 pertains.

[0023] The following describes in detail, with reference to the accompanying drawings, a specific scheme for preparing an organic polymer flocculant for water treatment provided in this application.

[0024] Specifically, one embodiment of this application provides a method for preparing an organic polymeric flocculant for water treatment. Please refer to [link to relevant documentation]. Figure 1 The method includes the following steps: Example 1 S1, by weight, 11 parts of acrylic acid and 19 parts of tetramethylguanidine are added to the reactor, heated to 45°C, and stirred for 3 hours for neutralization reaction. After the reaction is completed, a tetramethylguanidine acrylate solution is obtained.

[0025] S2, under nitrogen conditions, 2 parts of sorbitan monooleate were fully dissolved in 50 parts of cyclohexane solution, followed by the addition of 23 parts of acrylamide, 0.5 parts of vinylguanidine, and 5 parts of synergist. The mixture was heated to 45°C and stirred to obtain a mixed solution.

[0026] S3: Add the prepared mixture solution to the tetramethylguanidine acrylate solution neutralized in S1, then add 1 part of initiator and stir to carry out the polymerization reaction. The temperature is raised to 50°C by a heating device. By controlling and adjusting the reaction temperature during the polymerization process, the organic polymer flocculant is finally obtained.

[0027] The flowchart of the method for controlling and adjusting the reaction temperature during the polymerization process is attached. Figure 2 As shown, the details are as follows: S301 collects absorption spectral data of the polymerization reaction solution and reaction temperature data during the polymerization reaction.

[0028] Ten sampling points were uniformly selected within the polymerization reactor, and the absorption spectral data in the near-infrared wavelength range at each sampling point in the polymerization reaction solution were collected in real time using a Fourier transform infrared spectrometer. The vector composed of all the absorption spectral data at each sampling point in ascending order of wavelength was denoted as the absorbance vector at each sampling point.

[0029] Meanwhile, the reaction temperature at each sampling point in the polymerization reaction solution is collected in real time by a temperature sensor, with a sampling time interval of 10 seconds. The absorbance vector and reaction temperature at each sampling point at each sampling time are obtained. The implementer can adaptively select the number of sampling points and the sampling time interval according to the actual situation.

[0030] This embodiment utilizes a Fourier transform infrared spectrometer (FT-NIR) and a temperature sensor for data acquisition. FT-NIR spectrometers are generally equipped with fiber optic probes, which can be inserted into the reactor to measure the absorption spectrum data of the polymerization reaction solution in real time. The temperature sensor is a commonly used device for measuring the reaction temperature of the polymerization solution during the polymerization process, and can acquire the reaction temperature of the polymerization reaction solution in the reactor in real time.

[0031] S302, analyze the correlation between the reaction temperature and polymerization intensity characteristic values ​​at each sampling point in the polymerization reaction solution during each local sampling period, as well as the reaction temperature differences between sampling points, and determine the cumulative heat influence at each sampling point at each sampling time.

[0032] Typically, polymerization reactions involve exothermic processes, leading to localized heat accumulation in the polymerization solution. This localized heat accumulation results in excessively high reaction temperatures at specific locations within the polymerization solution, causing a rapid increase in the number of free radicals in the local reaction system and a higher probability of collisions between them. In this situation, the chain termination reaction rate exceeds the chain propagation reaction rate, leading to rapid termination of the polymerization reaction and ultimately affecting the intrinsic viscosity of the polymer product. Therefore, it is necessary to fully consider the characteristics of localized heat accumulation and accurately control and regulate the reaction temperature to reduce the adverse effects caused by localized heat accumulation in the polymerization solution and improve the intrinsic viscosity of the organic polymer flocculant after polymerization.

[0033] To analyze the polymerization intensity characteristics at various local locations in the polymerization reaction solution, the difference between the absorbance vector at each sampling point and the absorbance vector at the sampling point at each sampling time and the previous sampling time is calculated. The difference can be measured by DTW distance or Mahalanobis distance. In this embodiment, DTW distance is used to measure the difference. The greater the difference, the smaller the similarity between the two absorbance vectors, indicating that the polymerization change of organic molecules at that location is faster, reflecting that there is a higher reaction rate at that location in the polymerization reaction solution.

[0034] Simultaneously, the time difference between each acquisition moment and the previous acquisition moment is calculated, and the ratio of the difference to the time difference is recorded as the polymerization intensity characteristic value of each acquisition position at each acquisition moment. The polymerization intensity characteristic value reflects the polymerization intensity characteristics of organic molecules at local positions in the polymerization reaction solution. The larger the polymerization intensity characteristic value, the higher the polymerization intensity of organic molecules at local positions in the polymerization reaction solution.

[0035] Since the intensity characteristics of a polymerization reaction are affected not only by the reaction temperature but also by other polymerizing reactants, such as the initiator content and the total monomer mass fraction, the stronger the correlation between the polymerization intensity characteristics and the reaction temperature in a short period of time, the greater the influence of the reaction temperature on the polymerization process. Furthermore, the greater the difference between the reaction temperature at the sampling point and the reaction temperatures at other sampling points, the more it indicates that heat accumulation is occurring locally in the polymerization solution.

[0036] Furthermore, for each sampling point in the polymerization reaction solution, the reaction temperature and polymerization intensity characteristic values ​​of all sampling moments within a preset time period prior to each sampling moment are arranged in chronological order to obtain the reaction temperature sequence and polymerization intensity characteristic sequence for each sampling point at each sampling moment. The reaction temperature sequence and polymerization intensity characteristic sequence respectively reflect the changes in reaction temperature and polymerization intensity characteristics at local locations in the polymerization reaction solution. In this embodiment, the preset time period is 10 minutes, which can be set by the implementer.

[0037] Based on the above analysis, the cumulative heat impact at each sampling point at each sampling time was calculated: In the formula, Let J represent the cumulative heat influence at the j-th sampling point at the t-th sampling time. The correlation between the reaction temperature sequence and the polymerization intensity characteristic sequence at the j-th sampling point at the t-th sampling time can be measured using covariance or Pearson correlation coefficient. This embodiment uses covariance to measure the correlation. This represents the number of sampling points in the polymerization reaction solution. and These are the reaction temperatures at the j-th and s-th sampling points at the t-th sampling time, respectively.

[0038] The heat accumulation effect reflects the degree of influence of local heat accumulation in the polymerization reaction solution on the polymerization reaction. The greater the influence of local heat accumulation on the polymerization reaction, the less suitable the actual reaction temperature in the polymerization reaction solution is for the polymerization process. The more necessary it is to accurately control and adjust the reaction temperature of the polymerization reaction to avoid affecting the intrinsic viscosity of the organic polymer flocculant after the polymerization reaction.

[0039] S303. Based on the differences in the cumulative heat influence between all sampling points at each sampling time and the distance between the sampling points, and combined with the maximum value of the cumulative heat influence of all sampling points at each sampling time, the reliability of thermal imbalance at each sampling time is determined.

[0040] Meanwhile, the greater the difference in the degree of heat accumulation at different sampling points in the polymerization reaction solution, and the higher the degree of heat accumulation at local locations in the polymerization reaction solution, the more serious the local heat accumulation phenomenon in the polymerization reaction solution is. This will affect the heat balance of the polymerization reaction system and have an adverse effect on the intrinsic viscosity of the polymerization product. At this time, it is necessary to accurately control and adjust the reaction temperature of the polymerization reaction to ensure the effectiveness of the polymerization reaction and the intrinsic viscosity of the flocculant after the polymerization reaction.

[0041] Furthermore, the cumulative heat influence at each sampling point is arranged in ascending order to form a vector, which is denoted as the cumulative heat influence vector at each sampling point. The cumulative heat influence vector reflects the changes in the cumulative heat influence between different sampling points in the polymerization reaction solution. The greater the difference in the cumulative heat influence between different sampling points and the smaller the spatial distance between different sampling points, the clearer it is to indicate that the difference in the cumulative heat in the local area of ​​the polymerization reaction solution is more significant and more likely to affect the thermal stability of the polymerization reaction system.

[0042] Based on the above analysis, the significance of the difference in heat accumulation at each sampling time during the polymerization reaction was calculated: In the formula, The significance of the difference in heat accumulation at the t-th sampling time during the polymerization reaction is given. and These are the k-th and (k-1)-th elements in the heat accumulation influence vector at the t-th acquisition time, respectively. Let be the Euclidean distance between the locations of the sampling points corresponding to the k-th and (k-1)-th elements in the thermal cumulative influence vector at the t-th sampling time. The calculation of the Euclidean distance is a well-known technique, and the specific process will not be elaborated here.

[0043] The significance of heat accumulation difference reflects the degree of significance of heat accumulation difference in local areas of the polymerization reaction solution. The higher the significance of heat accumulation difference, the more serious the heat accumulation in local areas of the polymerization reaction solution, and the more likely it is to have a serious impact on the thermal stability of the polymerization reaction system, thus causing thermal imbalance in the polymerization reaction system. At this time, it is more necessary to accurately control and adjust the reaction temperature of the polymerization reaction to reduce the adverse effects of the reaction temperature on the intrinsic viscosity of the flocculant after the polymerization reaction.

[0044] Furthermore, the exponentially normalized result of the product of the significant difference in heat accumulation at each sampling moment and the maximum value of the heat accumulation influence at all sampling points at each sampling moment is denoted as the thermal imbalance characteristic value of the polymerization system at each sampling moment during the polymerization process. The thermal imbalance characteristic value reflects the magnitude of the heat imbalance in the polymerization system. The greater the heat imbalance in the polymerization system, the more unsuitable the actual polymerization temperature is for the polymerization process, and the more accurate the control and adjustment of the polymerization temperature is required.

[0045] Meanwhile, if the thermal imbalance characteristics show a continuous upward trend in the historical time prior to the current acquisition time, it indicates that the reliability of the thermal imbalance in the polymerization reaction system at this time is higher, which is more conducive to the accurate control and adjustment of the reaction temperature in the polymerization reaction system in the future.

[0046] Therefore, the thermal imbalance characteristic values ​​of all acquisition times within the preset time period prior to the current acquisition time are arranged in chronological order and denoted as the thermal imbalance characteristic vector of the current acquisition time. The first-order difference vector of the thermal imbalance characteristic vector is then calculated. This first-order difference vector reflects the changing characteristics of thermal imbalance over the historical time period prior to the current acquisition time. The ratio of the number of all positive elements in the first-order difference vector to the total number of elements is then calculated. The larger the ratio, the more pronounced the upward trend of thermal imbalance over historical time. Simultaneously, the mean of all positive elements within the first-order difference vector is calculated. The larger the mean value, the higher the value of the thermal imbalance characteristics over a historical period, indicating a higher degree of reliability of the thermal imbalance in the polymerization reaction system at this time.

[0047] Furthermore, the ratio with the mean The product of the two values ​​is denoted as the confidence weight at the current acquisition time. The exponentially normalized result of the product of the confidence weight at the current acquisition time and the thermal imbalance characteristic value at the current acquisition time is denoted as the thermal imbalance confidence at the current acquisition time. The thermal imbalance confidence reflects the degree of confidence of the thermal imbalance state during the polymerization reaction. The higher the confidence, the more likely thermal imbalance will occur in the polymerization reaction system. At this time, it is necessary to accurately control and adjust the reaction temperature of the polymerization reaction.

[0048] S304. Based on the difference between the thermal imbalance confidence level and its segmentation threshold, and the actual reaction temperature obtained from the average reaction temperature at all sampling points, the expected reaction temperature at the current sampling moment is obtained. The PID controller is used to control and adjust the reaction temperature during the polymerization process based on the temperature error between the expected reaction temperature and the actual reaction temperature.

[0049] Furthermore, in order to accurately control and adjust the reaction temperature during the polymerization process, the thermal imbalance confidence levels of all historical acquisition times prior to the current acquisition time are input into the Otsu's inter-class variance algorithm. The Otsu's inter-class variance algorithm is used to obtain the segmentation threshold of the thermal imbalance confidence level. The Otsu's inter-class variance algorithm is a well-known technique, and the specific process will not be described in detail.

[0050] If the reliability of thermal imbalance at the current sampling moment during the polymerization reaction is higher than the segmentation threshold, it indicates that thermal imbalance has occurred in the polymerization solution. In this case, the reaction temperature should be lowered to avoid affecting the intrinsic viscosity of the polymerization product. Conversely, if the reliability of thermal imbalance at the current sampling moment during the polymerization reaction is lower than the segmentation threshold, it indicates that thermal imbalance has not occurred in the polymerization solution. In this case, the reaction temperature should be increased to enhance the activity of the monomers and avoid adverse effects on the formation of the polymerization product.

[0051] Based on the above analysis, the average reaction temperature at all sampling points at the current sampling time is recorded as the actual reaction temperature at the current sampling time, and the expected reaction temperature at the current sampling time during the polymerization process is calculated: In the formula, This represents the desired reaction temperature at the current sampling moment during the polymerization process. This represents the actual reaction temperature at the current sampling moment. To assess the reliability of the thermal imbalance at the current sampling moment during the polymerization reaction. This is the threshold for determining the reliability of thermal imbalance during the historical process of the polymerization reaction. The historical process consists of all acquisition times prior to the current acquisition time.

[0052] Therefore, by adjusting the actual reaction temperature based on the reliability of thermal imbalance during the polymerization reaction, the desired reaction temperature can be obtained, avoiding the adverse effects of excessively high or low reaction temperatures on the polymerization reaction, thereby ensuring the effectiveness of the polymerization reaction and the intrinsic viscosity of the flocculant after the polymerization reaction.

[0053] Furthermore, the reaction temperature during the polymerization process is accurately controlled and regulated by a PID controller. The actual reaction temperature and the desired reaction temperature at the current acquisition moment during the polymerization process are transmitted to the PID controller. The PID controller inputs a control signal for the reaction temperature based on the temperature error between the actual reaction temperature and the desired reaction temperature, and transmits the control signal for the reaction temperature to the heating device. The heating device controls the actual reaction temperature during the polymerization process to approach the desired reaction temperature, thereby achieving accurate control and regulation of the reaction temperature during the polymerization process.

[0054] Example 2 S1, by weight, 14 parts of acrylic acid and 27 parts of tetramethylguanidine are added to the reactor, heated to 60°C, and stirred for 5 hours for neutralization reaction. After the reaction is completed, a tetramethylguanidine acrylate solution is obtained.

[0055] S2, under nitrogen conditions, 4 parts of sorbitan monooleate were fully dissolved in 100 parts of cyclohexane solution, followed by the addition of 27 parts of acrylamide, 1 part of vinylguanidine, and 12 parts of synergist. The mixture was heated to 60°C and stirred to obtain a mixed solution.

[0056] S3: Add the prepared mixture solution to the tetramethylguanidine acrylate solution neutralized in S1, then add 5 parts of initiator and stir to carry out the polymerization reaction. The temperature is raised to 50°C by a heating device. By controlling and adjusting the reaction temperature during the polymerization process, the organic polymer flocculant is finally obtained.

[0057] In this embodiment, the method for controlling and adjusting the reaction temperature during the polymerization process is the same as that in Example 1.

[0058] Example 3 S1, by weight, 13 parts of acrylic acid and 24 parts of tetramethylguanidine are added to the reactor, heated to 55°C, and stirred for 4 hours for neutralization reaction. After the reaction is completed, a tetramethylguanidine acrylate solution is obtained.

[0059] S2, under nitrogen conditions, 3 parts of sorbitan monooleate were fully dissolved in 80 parts of cyclohexane solution, followed by the addition of 25 parts of acrylamide, 0.75 parts of vinylguanidine, and 9 parts of synergist. The mixture was heated to 55°C and stirred to obtain a mixed solution.

[0060] S3: Add the prepared mixture solution to the tetramethylguanidine acrylate solution neutralized in S1, then add 3 parts of initiator and stir to carry out the polymerization reaction. The temperature is raised to 50°C by a heating device. By controlling and adjusting the reaction temperature during the polymerization process, the organic polymer flocculant is finally obtained.

[0061] In this embodiment, the method for controlling and adjusting the reaction temperature during the polymerization process is the same as that in Example 1.

[0062] The above technical features constitute the preferred embodiment of this application, which has strong adaptability and the best implementation effect. Unnecessary technical features can be added or removed according to actual needs to meet the needs of different situations.

Claims

1. A method for preparing an organic polymeric flocculant for water treatment, characterized in that, The method comprises the following steps: S1, according to the weight part, 11-14 parts of acrylic acid and 19-27 parts of tetramethyl guanidine are added into the reactor, heated and stirred to obtain a tetramethyl guanidine acrylic acid solution; S2, under the condition of nitrogen, 2-4 parts of sorbitan monooleate are fully dissolved in 50-100 parts of cyclohexane solution, then 23-27 parts of acrylamide, 0.5-1 part of vinyl guanidine amine, 5-12 parts of synergist are added, and the mixture solution is obtained by heating and stirring; S3, the tetramethyl guanidine acrylic acid solution and the mixture solution are mixed, then the initiator is added and the polymerization reaction is carried out by stirring, and the reaction temperature in the polymerization reaction process is controlled and adjusted, and finally the organic high molecular flocculant is obtained; The control and adjustment method is: S301, the absorption spectrum data and the reaction temperature data of the polymerization reaction solution in the polymerization reaction process are collected; S302, the correlation between the reaction temperature and the polymerization intensity characteristic value of each collection point position in each local collection period, and the reaction temperature difference between the collection point positions are analyzed, and the heat accumulation influence degree of each collection point position at each collection time is determined; S303, according to the heat accumulation influence degree difference between all collection point positions at each collection time and the distance between the positions, and combining the maximum value of the heat accumulation influence degree of all collection point positions at each collection time, the heat imbalance credibility of each collection time is determined; S304, according to the difference between the heat imbalance credibility and its segmentation threshold value, and the actual reaction temperature obtained by the mean value of the reaction temperature of all collection point positions, the expected reaction temperature of the current collection time is obtained, and the reaction temperature in the polymerization reaction process is controlled and adjusted based on the temperature error between the expected reaction temperature and the actual reaction temperature by using the PID controller.

2. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, In step S1, the heating temperature is 45-60℃, and the stirring time is 3-5h for neutralization reaction, and the tetramethyl guanidine acrylic acid solution is obtained after the neutralization reaction is completed.

3. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, The temperature of the temperature rise in step S2 is 45-60℃.

4. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, The weight part of the initiator added in step S3 is 1-5 parts.

5. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, The acquisition method of the polymerization intensity characteristic value is: The difference between the absorbance vector at each collection point position at each collection time and the last collection time is calculated; The ratio of the difference degree to the time difference is recorded as the polymerization intensity characteristic value of each collection position at each collection time.

6. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, The determination method of the heat imbalance credibility is: According to the heat accumulation influence degree difference between all collection point positions at each collection time and the distance between the positions, the heat accumulation difference significance of each collection time is determined; The exponential normalization result of the product of the heat accumulation difference significance of each collection time and the maximum value of the heat accumulation influence degree of all collection point positions at each collection time is recorded as the heat imbalance characteristic value of the polymerization reaction system at each collection time in the polymerization reaction process; A vector composed of the thermal imbalance feature values of all collection time points in a preset period before the current collection time in time sequence is recorded as a thermal imbalance feature vector of the current collection time, and a first-order difference vector of the thermal imbalance feature vector is calculated; the ratio of the number of positive elements within the statistical first difference vector to the total number of elements ; computing the mean of all positive valued elements within the first difference vector ; the ratio the product of the mean value is recorded as the credibility weight value of the current acquisition time, and the exponential normalization result of the product of the credibility weight value of the current acquisition time and the thermal imbalance feature value of the current acquisition time is recorded as the thermal imbalance credibility of the current acquisition time.

7. The method for preparing an organic polymeric flocculant for water treatment as described in claim 6, characterized in that, The determination method of the thermal accumulation difference significance of each collection time point is: A sequence is composed of the heat accumulation influence degrees of all collection point positions at each collection time point in ascending order; For any two adjacent elements in the sequence, the numerical difference between the adjacent next element and the previous element is calculated, the Euclidean distance of the corresponding collection point positions of the adjacent next element and the previous element is calculated, and the ratio of the numerical difference to the Euclidean distance is calculated; The sum of the ratios calculated between all adjacent elements in the sequence is taken as the thermal accumulation difference significance of each collection time point.

8. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, The acquisition method of the reaction expected temperature of the current collection time point is: The mean value of the reaction temperature at all collection point positions at the current collection time point is recorded as the actual reaction temperature of the current collection time point. wherein is the expected reaction temperature at the current acquisition time point in the polymerization process, is the actual reaction temperature at the current acquisition time point, is the thermal imbalance reliability at the current acquisition time point in the polymerization process, is the split threshold of the thermal imbalance reliability in the historical process of the polymerization; the historical process is composed of all acquisition time points before the current acquisition time point.

9. The method of claim 8, wherein the organic polymer flocculant is prepared by the steps of: (a) mixing the monomers in the presence of the initiator; (b) polymerizing the monomers; (c) adding the polymer to the water; and (d) adding the coagulant to the water. The acquisition method of the segmentation threshold is: inputting the thermal imbalance confidence of all collection time points in the historical process into the maximum inter-class variance algorithm, and using the maximum inter-class variance algorithm to obtain the segmentation threshold of the thermal imbalance confidence.

10. The method for preparing an organic polymeric flocculant for water treatment as described in claim 1, characterized in that, The control and adjustment of the reaction temperature in the polymerization reaction process based on the temperature error between the reaction expected temperature and the actual reaction temperature by the PID controller includes: The actual reaction temperature and the reaction expected temperature of the current collection time point in the polymerization reaction process are transmitted to the PID controller, the PID controller inputs the control signal of the reaction temperature through the temperature error between the actual reaction temperature and the reaction expected temperature, and transmits the control signal of the reaction temperature to the heating device, so as to control the actual reaction temperature in the polymerization reaction process to approach the reaction expected temperature by the heating device.

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