Preparation method of quick-drying water-based ink resin

By using pre-emulsification control module and polymerization control module in the preparation process of aqueous ink resin, the precise mixing and polymerization reaction conditions of emulsified raw materials are achieved, and the problems of unstable product quality and slow drying speed in the prior art are solved, and the production efficiency and product quality are improved.

CN120209202AInactive Publication Date: 2025-06-27TIANJIN JUSHI NEW MATERIAL TECH CO LTD

Patent Information

Application Number
CN202510354137.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-25
Publication Date
2025-06-27
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing water-based ink resin preparation process is difficult to accurately control the parameters of each link, resulting in unstable product quality and slow drying speed, limiting its application in efficient printing scenarios.

Method used

The pre-emulsification control module and the polymerization control module are adopted to accurately mix emulsification raw materials and control polymerization reaction conditions through preset ratios and real-time regulation. The conversion rate is monitored in real time by using near-infrared spectroscopy to ensure high-quality preparation of emulsions and resins.

Benefits of technology

The quality of pre-emulsions and resins is improved, the efficiency of polymerization and the stability of products are ensured, the production efficiency and product quality are improved, and the quality is suitable for the high-quality and rapid delivery needs of the modern printing industry.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of ink resin preparation, in particular to a preparation method of quick-dry water-based ink resin.The preparation method comprises the steps that a pre-emulsification control module drives all emulsification raw material storage devices according to a preset proportion, pre-emulsification raw materials are injected into an emulsification kettle according to a certain sequence, the pre-emulsification technological process is regulated and controlled in real time, and pre-emulsion is prepared; a polymerization control module is used for adding part of the pre-emulsion and the polymerization initiator solution into a polymerization reaction kettle, when the polymerization reaction reaches a certain degree, the remaining pre-emulsion and the polymerization initiator solution are synchronously added according to a certain proportion, and polymerization is finished after the conversion rate is monitored to reach the standard in real time through near infrared spectroscopy. According to the present invention, through the preset ratio and the real-time regulation, the accurate mixing of the emulsification raw material and the strict control of the reaction condition can be ensured so as to improve the quality of the pre-emulsion and lay the good foundation for the subsequent polymerization reaction.
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Description

Technical Field

[0001] The present invention relates to the technical field of ink resin preparation, and particularly relates to a preparation method of a quick-drying water-based ink resin. Background Art

[0002] In the field of water-based ink resin preparation, in the traditional process, it is difficult to accurately control the parameters of each link, resulting in uneven product quality. The particularly prominent problem is the slow drying speed, which severely restricts its application in high-efficiency printing scenarios. In traditional manual or semi-automatic operations, the raw material ratio error is large, and the reaction conditions fluctuate frequently. It is impossible to ensure that the performance of each batch of resin is consistent, resulting in long drying time for printed products, low production efficiency, and quality defects such as ink layer adhesion and color deviation caused by poor drying. With the progress of automation and sensing technologies, the introduction of intelligent control systems provides an opportunity to break through the bottleneck. By real-time and accurately monitoring and regulating the reaction conditions, it is expected to stably produce high-performance quick-drying water-based ink resins, which can not only greatly improve production efficiency but also ensure highly stable product quality, meeting the urgent needs of the modern printing industry for high quality and fast delivery.

[0003] Chinese Patent Publication No.: CN104629525A discloses a preparation method of a water-based ink binder composed of a composite of an inorganic material and a water-based amino resin, including the thermal activation, acid activation, and silane coupling agent modification of halloysite and sepiolite, and then compounding the obtained modified inorganic material with the water-based amino resin to obtain the water-based ink binder composed of the composite of the inorganic material and the water-based amino resin.

[0004] Differences in manufacturer batches of chemical products can lead to different reaction speeds and finished product qualities of the products. In the current ink preparation process, raw materials are often put in and prepared according to preset ratios and processes, lacking intelligent control during the preparation process, resulting in uneven product quality. Summary of the Invention

[0005] Therefore, the present invention provides a preparation method of a quick-drying water-based ink resin to overcome the problems in the prior art that differences in manufacturer batches of chemical products can lead to different reaction speeds and finished product qualities of the products, and in the current ink preparation process, raw materials are often put in and prepared according to preset ratios and processes, lacking intelligent control during the preparation process, resulting in uneven product quality.

[0006] To achieve the above object, the present invention provides a preparation method of a quick-drying water-based ink resin, including:

[0007] The pre-emulsification control module drives each emulsified raw material storage device according to a preset ratio, injects the pre-emulsified raw materials into the emulsification kettle in a certain order, and real-time regulates the pre-emulsification process to prepare a pre-emulsion;

[0008] The polymerization control module adds a part of the pre-emulsion and the polymerization initiator solution into the polymerization reactor. When the polymerization reaction reaches a certain degree, the remaining pre-emulsion and the polymerization initiator solution are added synchronously in a certain proportion, and the polymerization ends after the conversion rate is monitored in real time by near-infrared spectroscopy and reaches the standard;

[0009] A cross-linking agent is added to the polymerized mixture to prepare a crude resin;

[0010] The prepared crude resin is cooled to room temperature and pH neutralized, and the product is filtered and then stored;

[0011] When preparing the pre-emulsion, the pre-prepared mixed monomers are gradually added to the emulsion matrix, and during the dropping process of the mixed monomers, the preparation process of the emulsifying kettle is regulated by on-line monitoring with a viscosity sensor and a laser particle size analyzer.

[0012] Further, the order of adding the pre-emulsified raw materials to the emulsifying kettle is:

[0013] The non-ionic emulsifier octylphenol polyoxyethylene ether and the anionic emulsifier sodium dodecyl sulfate are added to deionized water in a mass ratio of 1:1 and a total amount of 2.5% of the total mass of the monomers, and the stirring equipment is started for stirring to prepare an emulsion matrix;

[0014] After the stirring equipment runs smoothly, the mixed monomers are prepared by mixing methyl methacrylate, butyl acrylate, and hydroxyethyl acrylate in a mass ratio of 3:2:1, and are added dropwise to the emulsifying kettle by a peristaltic pump at a preset speed;

[0015] During the dropping process of the mixed monomers, on-line monitoring is carried out with a viscosity sensor and a laser particle size analyzer, and the dropping speed of the peristaltic pump is regulated in real time according to the monitoring results.

[0016] Further, the pre-emulsification control module determines the first regulation information variable according to the data collected by the viscosity sensor, determines the second regulation information variable according to the data collected by the laser particle size analyzer, and the pre-emulsification control module regulates the preparation process of the emulsifying kettle through the first regulation information variable and the second regulation information variable.

[0017] Further, the viscosity sensor monitors the viscosity of the mixed solution in the emulsifying kettle in real time and transmits the monitoring results to the pre-emulsification control module. The pre-emulsification control module generates a viscosity change curve according to the monitored data. A standard viscosity change curve is set in the pre-emulsification control module, and the pre-emulsification control module determines the first regulation information variable according to the relationship between the generated viscosity change curve and the standard viscosity change curve.

[0018] Furthermore, the laser particle size analyzer monitors the distribution uniformity of the mixed solution in the emulsifying kettle in real time and transmits the monitoring results to the pre-emulsification control module. The pre-emulsification control module generates a distribution uniformity change curve based on the monitored data. A standard distribution uniformity change curve is set in the pre-emulsification control module, and the pre-emulsification control module determines the second regulation information variable according to the relationship between the generated distribution uniformity change curve and the standard distribution uniformity change curve.

[0019] Furthermore, the first regulation information variable is determined through comprehensive evaluation among the viscosity change dispersion degree, the viscosity change slope, and the viscosity average value. Furthermore, when the average value of the generated distribution uniformity change curve is greater than or equal to the average value of the standard distribution uniformity change curve, the pre-emulsification control module regulates the preparation process of the emulsifying kettle only through the first regulation information variable.

[0020] Furthermore, the dosage of the polymerization initiator solution is 0.8% of the total mass of the monomers, which is ammonium persulfate prepared into a 10% aqueous solution.

[0021] Furthermore, during the polymerization reaction, first pump 1 / 3 of the pre-emulsion into the reaction kettle, add the initiator solution, heat the reaction kettle to 70 °C, and adjust the stirring speed to 900 r / min. Maintain this temperature to initiate polymerization for 30 minutes, during which blue light appears initially; subsequently, synchronously dropwise add the remaining pre-emulsion and the initiator solution according to the set curve to ensure a stable reaction at 75 - 80 °C for 2.5 hours, and end the polymerization when the conversion rate is monitored in real time by near-infrared spectroscopy and exceeds 90%.

[0022] Furthermore, after the polymerization is completed, adjust the stirring speed to 700 r / min, adjust the temperature to 60 °C, add an aziridine cross-linking agent, and introduce ammonia gas to maintain the pH value at 7 - 8 for cross-linking reaction.

[0023] Compared with the prior art, the beneficial effects of the present invention are that through preset ratios and real-time regulation, it is possible to ensure the precise mixing of the emulsifying raw materials and the strict control of the reaction conditions, thereby improving the quality of the pre-emulsion and laying a good foundation for the subsequent polymerization reaction. The polymerization control module can effectively control the process of the polymerization reaction by precisely controlling the addition ratio and timing of the polymerization initiator and by monitoring the conversion rate in real time through near-infrared spectroscopy, ensuring the high efficiency of the polymerization reaction and the quality of the product.

[0024] Furthermore, by adding a crosslinking agent, the crosslinking density and stability of the resin can be enhanced, thereby improving the mechanical properties and chemical resistance of the resin, providing a basis for the preparation of high-performance fast-drying waterborne ink resin. Cooling the resin to room temperature and neutralizing the pH can avoid the influence of high temperature on the resin properties and ensure the stability of the resin through pH adjustment. Storage after filtration can remove impurities and ensure the purity and quality of the resin product. Adding emulsifier and deionized water in a specific order and proportion can ensure the uniform dispersion of the emulsifier, providing a good basis for the dropping of mixed monomers and the formation of emulsion, thereby improving the stability and quality of the emulsion.

[0025] Furthermore, through on-line monitoring by a viscosity sensor and a laser particle size analyzer, the preparation status of the emulsion matrix can be understood in real time, and by regulating the dropping speed of the peristaltic pump, precise control of the emulsification process can be achieved, thereby improving the uniformity and stability of the emulsion.

[0026] Furthermore, the pre-emulsification control module can generate a change curve by collecting viscosity and particle size data and compare it with the standard curve, and can adjust the emulsification process in real time to ensure the quality and stability of the emulsion, providing a guarantee for the preparation of high-quality fast-drying waterborne ink resin. The real-time monitoring by the viscosity sensor and the laser particle size analyzer can provide accurate data on the emulsion preparation status, which are crucial for the pre-emulsification control module and help the control module make correct regulation decisions to ensure the uniformity and stability of the emulsion.

[0027] Furthermore, by determining the regulation weight according to the data relationship between the first regulation information variable (viscosity) and the second regulation information variable (particle size), more refined control of the preparation process can be achieved, the preparation conditions of the emulsion can be optimized, and the product quality can be improved. When the average value of the change curve of the distribution uniformity is greater than or equal to the average value of the standard change curve of the distribution uniformity, the pre-emulsification control module only regulates through viscosity, which can reduce unnecessary regulation actions, improve the preparation efficiency, and ensure the uniformity and stability of the emulsion at the same time.

[0028] By obtaining the dispersion degree of the viscosity change curve, the viscosity change situation can be analyzed. When the viscosity changes evenly, it indicates that the process during pre-emulsification is stable, and the data shown is a smaller value of the dispersion degree. While a larger value of the dispersion degree indicates that the emulsification process is unstable during stirring, and the greater the value, the greater this instability. Therefore, the calculation compensation parameter of the first regulation information variable is determined through the dispersion degree to ensure the accurate calculation of the first regulation information variable and guarantee the calculation accuracy of the overall regulation data.

[0029] During the emulsification process, the viscosity changes in real time. By analyzing the viscosity curve, its slope is determined and compared with the corresponding standard slope within the same time period. If the slope of the reaction is not much different from the standard slope, it indicates that the reaction rate at this time is basically the same as the ideal reaction rate. Otherwise, it means there is a deviation between the reaction rate and the ideal rate. The greater the difference from the standard rate, the greater the deviation. Therefore, the greater the deviation, the greater the influence parameter of the set slope difference.

[0030] During the pre-emulsification process, the average value of the viscosity reflects the overall degree of emulsification. If the value of the viscosity is relatively close to the standard data, it indicates that the pre-emulsification process is similar to the preset standard process. Otherwise, it means there is a large difference. The greater the difference from the standard average value, the greater the deviation. Therefore, the greater the deviation, the greater the influence parameter of the set average value.

[0031] Through the comprehensive evaluation among the viscosity change dispersion, viscosity change slope, and viscosity average value during the stirring process, the actual situation of the viscosity during the pre-emulsification process is determined, and the specific value of the first regulation information variable is determined. The comprehensive evaluation prevents the deviation of a single data evaluation from affecting the overall regulation situation and ensures the accuracy of the evaluation of the pre-emulsification process.

[0032] The higher the distribution uniformity, the smoother the change in uniformity during the stirring process. Otherwise, it means it is less smooth. For cases greater than the preset uniformity, it indicates that it is better than the preset situation, so it is not used as the influencing data for real-time regulation of the process. For cases less than the preset situation, the greater the difference from the preset situation, the greater the difference from the standard situation, and the more regulation is needed. Therefore, the greater the value of the corresponding second regulation information variable to ensure the accuracy of the regulation process.

[0033] The pre-emulsification process is comprehensively determined through the viscosity data and the particle size distribution uniformity, ensuring the accuracy of the evaluation result. At the same time, by setting different intervals, different adjustments are made to the pre-emulsification to ensure the accuracy of the regulation. For those with small differences, no adjustment is made to maintain the stability of the pre-emulsification process. For those with medium differences, the rotation speed is adjusted to ensure that the pre-emulsification reaches the standard interval as soon as possible without destroying the ratio. For those with large differences, the raw material addition speed is adjusted to regulate the reaction situation of the pre-emulsification so that it can fit the standard reaction as soon as possible. Description of the Drawings

[0034] Figure 1 It is a schematic flow chart of the preparation method of the fast-drying water-based ink resin in the embodiment;

[0035] Figure 2 It is a schematic flow chart for determining the first regulation information variable in the embodiment;

[0036] Figure 3 It is a schematic flow chart for determining the second regulation information variable in the embodiment. Detailed implementation manners

[0037] In order to make the objectives and advantages of the present invention clearer and more understandable, the present invention will be further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0038] The preferred implementation manners of the present invention will be described below with reference to the accompanying drawings. Those skilled in the art should understand that these implementation manners are only used to explain the technical principles of the present invention and do not limit the protection scope of the present invention.

[0039] It should be noted that in the description of the present invention, the terms indicating the direction or positional relationship such as "upper", "lower", "left", "right", "inner", "outer", etc. are based on the direction or positional relationship shown in the drawings. This is only for convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

[0040] In addition, it should also be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installation", "connection", and "coupling" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

[0041] Please refer to Figures 1 - 3 as shown Figure 1 is a schematic flow chart of the preparation method of the quick-drying water-based ink resin in the embodiment; Figure 2 is a schematic flow chart for determining the first regulation information variable in the embodiment; Figure 3 is a schematic flow chart for determining the second regulation information variable in the embodiment.

[0042] The present invention provides a preparation method of a quick-drying water-based ink resin, including,

[0043] S1. The pre-emulsification control module drives each emulsifying raw material storage device according to a preset ratio, injects the pre-emulsifying raw materials into the emulsifying kettle in a certain order, and performs real-time regulation on the pre-emulsification process to prepare a pre-emulsion;

[0044] S2. The polymerization control module adds part of the pre-emulsion and the polymerization initiator solution into the polymerization reaction kettle. When the polymerization reaction reaches a certain degree, the remaining pre-emulsion and the polymerization initiator solution are added synchronously in a certain proportion, and the polymerization ends after the conversion rate is monitored in real time by near-infrared spectroscopy and reaches the standard;

[0045] S3. Add a crosslinking agent to the mixture after the aggregation is completed to prepare a crude resin;

[0046] S4. Cool the prepared crude resin to room temperature and carry out pH neutralization. After filtration, the product is stored;

[0047] When preparing the pre-emulsion, the pre-prepared mixed monomers are gradually added to the emulsion matrix. During the dropping process of the mixed monomers, the preparation process of the emulsification kettle is regulated through on-line monitoring by a viscosity sensor and a laser particle size analyzer.

[0048] Through the preset ratio and real-time regulation, the precise mixing of the emulsification raw materials and the strict control of the reaction conditions can be ensured, thereby improving the quality of the pre-emulsion and laying a good foundation for the subsequent polymerization reaction. The polymerization control module can effectively control the process of the polymerization reaction and ensure the high efficiency of the polymerization reaction and the quality of the product by precisely controlling the addition ratio and timing of the polymerization initiator and by real-time monitoring the conversion rate through near-infrared spectroscopy.

[0049] Specifically, the order of adding the pre-emulsified raw materials to the emulsification kettle is as follows:

[0050] Add non-ionic emulsifier octylphenol polyoxyethylene ether and anionic emulsifier sodium dodecyl sulfate to deionized water at a mass ratio of 1:1 and a total amount of 2.5% of the total mass of the monomers, and start the stirring equipment to stir to prepare an emulsion matrix;

[0051] After the stirring equipment runs smoothly, prepare a mixed monomer by mixing methyl methacrylate, butyl acrylate, and 2-hydroxyethyl acrylate at a mass ratio of 3:2:1, and add it dropwise to the emulsification kettle by a peristaltic pump at a preset speed;

[0052] During the dropping process of the mixed monomers, on-line monitoring is carried out by a viscosity sensor and a laser particle size analyzer, and the dropping speed of the peristaltic pump is regulated according to the monitoring results.

[0053] By adding a crosslinking agent, the crosslinking density and stability of the resin can be enhanced, thereby improving the mechanical properties and chemical resistance of the resin and providing a basis for preparing a high-performance fast-drying water-based ink resin. Cooling the crude resin to room temperature and carrying out pH neutralization can avoid the influence of high temperature on the resin performance and ensure the stability of the resin through pH adjustment. Filtration and storage can remove impurities and ensure the purity and quality of the resin product. Adding emulsifiers and deionized water in a specific order and ratio can ensure the uniform dispersion of the emulsifiers, provide a good basis for the dropping of the mixed monomers and the formation of the emulsion, and thus improve the stability and quality of the emulsion.

[0054] Specifically, the pre-emulsification control module determines the first regulation information variable according to the data collected by the viscosity sensor, and determines the second regulation information variable according to the data collected by the laser particle size analyzer. The pre-emulsification control module regulates the preparation process of the emulsification kettle through the first regulation information variable and the second regulation information variable.

[0055] Through on-line monitoring by the viscosity sensor and the laser particle size analyzer, the preparation state of the emulsion matrix can be understood in real time, and by regulating the dropping speed of the peristaltic pump, precise control of the emulsification process can be achieved, thereby improving the uniformity and stability of the emulsion.

[0056] Specifically, the viscosity sensor monitors the viscosity of the mixed solution in the emulsification kettle in real time, and transmits the monitoring result to the pre-emulsification control module. The pre-emulsification control module generates a viscosity change curve according to the monitored data. A standard viscosity change curve is set in the pre-emulsification control module, and the pre-emulsification control module determines the first regulation information variable according to the relationship between the generated viscosity change curve and the standard viscosity change curve.

[0057] The pre-emulsification control module records the generated viscosity change curve as F(1) and the standard viscosity change curve as F(0);

[0058] A comparison duration T is set in the pre-emulsification control module. When the abscissa of the viscosity change curve F(1) reaches the comparison duration T, the pre-emulsification control module analyzes the viscosity change curve F(1), including,

[0059] Connect the starting point and the ending point of the viscosity change curve F(1) within the comparison duration T to generate the first analysis straight line L1;

[0060] The pre-emulsification control module analyzes the dispersion degree of the viscosity change curve F(1) relative to the first analysis straight line L1 to determine the first dispersion degree value;

[0061] A standard dispersion degree value is set in the pre-emulsification control module,

[0062] If the first dispersion degree value is less than or equal to the standard dispersion degree value, the calculation compensation parameter of the first regulation information variable is 1;

[0063] If the first dispersion degree value is greater than the standard dispersion degree value, the pre-emulsification control module determines the calculation compensation parameter of the first regulation information variable according to the difference between the first dispersion degree value and the standard dispersion degree value; the value of the calculation compensation parameter of the first regulation information variable is positively correlated with the difference between the first dispersion degree value and the standard dispersion degree value, and the value is greater than 1.

[0064] By obtaining the dispersion degree of the viscosity change curve, the viscosity change situation can be analyzed. When the viscosity changes evenly, it indicates that the pre-emulsification process is stable, and the data presented is that the value of the dispersion degree is small. While a large value of the dispersion degree indicates that the emulsification process during stirring is unstable, and the greater the value, the greater this instability. Therefore, the calculation compensation parameter of the first regulation information variable is determined through the degree of dispersion, ensuring the accuracy of the calculation of the first regulation information variable and guaranteeing the calculation accuracy of the overall regulation data.

[0065] For the viscosity change curve F(1), the pre-emulsification control module fits it into a second analysis straight line L2 through a linear regression model, obtains the curve segment of the corresponding standard viscosity change curve F(0) within the same comparison time period, and fits it into a standard straight line L0.

[0066] The pre-emulsification control module analyzes the slope difference between the second analysis straight line L2 and the standard straight line L0, and compares it with the standard slope difference interval.

[0067] If the slope difference falls within the standard slope difference interval, it is determined that the slope difference influence parameter is 1.

[0068] If the slope difference does not fall within the standard slope difference interval, the slope difference influence parameter is determined by the absolute value of the difference between the slope difference and the median of the standard slope difference interval, defined as the first absolute difference value. The greater the first absolute difference value, the greater the slope difference influence parameter, and the value is greater than 1.

[0069] During the emulsification process, the viscosity changes in real time. By analyzing the viscosity curve, its slope is determined, and compared with the standard slope that should correspond within the same time period. If the slope of the reaction is not much different from the standard slope, it indicates that the reaction rate at this time is basically the same as the ideal reaction rate. Otherwise, it indicates that there is a deviation between the reaction rate and the ideal rate. The greater the difference from the standard rate, the greater the deviation. Therefore, the greater the deviation, the greater the slope difference influence parameter set.

[0070] The pre-emulsification control module analyzes the average value of the viscosity change curve F(1), and analyzes the standard average value of the curve segment of the corresponding standard viscosity change curve F(0). The pre-emulsification control module calculates the absolute value of the difference between the average value of the viscosity change curve F(1) and the standard average value, defined as the absolute value of the average difference, and compares it with the standard absolute value of the average difference interval.

[0071] If the absolute value of the average difference falls within the standard absolute value of the average difference interval, it is determined that the average influence parameter is 1.

[0072] If the absolute value of the average difference does not fall into the standard average difference absolute value interval, the absolute value of the difference between the average value of the viscosity change curve F(1) and the median of the standard average difference absolute value interval is calculated, which is defined as the second absolute value of the difference. The larger the second absolute value of the difference, the greater the average influence parameter, and the value is greater than 1.

[0073] During the pre-emulsification process, the average value of viscosity reflects the overall degree of emulsification. If the viscosity value is slightly different from the standard data, it means that the pre-emulsification process is similar to the preset standard process. Otherwise, it means that the difference is large. The greater the difference from the standard average value, the greater the deviation. Therefore, the greater the deviation, the greater the impact of the set average value on the parameter.

[0074] Specifically, the first control information variable is determined by a comprehensive evaluation of the viscosity change dispersion, the viscosity change slope, and the viscosity average value.

[0075] The pre-emulsification control module determines the first control information variable by calculating the product of a calculation compensation parameter of the first control information variable, an average value influence parameter and a slope difference influence parameter.

[0076] Through comprehensive evaluation of the discreteness of viscosity change, the slope of viscosity change and the average viscosity during stirring, the actual situation of viscosity in the pre-emulsification process is determined, and the specific value of the first control information variable is determined. Comprehensive evaluation prevents the deviation of a single data evaluation from affecting the overall control situation, and ensures the accuracy of the pre-emulsification process evaluation.

[0077] Specifically, the laser particle size analyzer monitors the distribution uniformity of the mixed solution in the emulsification kettle in real time, and transmits the monitoring results to the pre-emulsification control module, the pre-emulsification control module generates a distribution uniformity change curve according to the monitored data, and a standard distribution uniformity change curve is provided in the pre-emulsification control module. The pre-emulsification control module determines the second control information variable according to the relationship between the generated distribution uniformity change curve and the standard distribution uniformity change curve.

[0078] The pre-emulsification control module determines the average value of the distribution uniformity change curve and compares it with the average value of the standard distribution uniformity.

[0079] If the average value of the obtained distribution uniformity change curve is greater than or equal to the average value of the standard distribution uniformity, it is determined that the distribution uniformity has no effect on the emulsification process;

[0080] If the average value of the obtained distribution uniformity change curve is less than the average value of the standard distribution uniformity, determine the value of the second regulation information variable according to the absolute value of the difference between the two. Set the absolute value of the difference between the average value of the obtained distribution uniformity change curve and the average value of the standard distribution uniformity as the third absolute value of the difference. The larger the third absolute value of the difference, the larger the value of the second regulation information variable.

[0081] The higher the distribution uniformity, the smoother the change in uniformity during the stirring process. Conversely, the less smooth it is. For cases greater than the preset uniformity, it indicates that it is better than the preset situation, so it is not used as the influencing data for real-time regulation of the process. For cases less than the preset situation, the larger the difference from the preset situation, the greater the difference from the standard situation, and the more regulation is needed. Therefore, the value of the corresponding second regulation information variable is larger, ensuring the accuracy of the regulation process.

[0082] The pre-emulsification control module can collect viscosity and particle size data, generate change curves, and compare them with the standard curves to adjust the emulsification process in real time, ensuring the quality and stability of the emulsion, and providing guarantee for the preparation of high-quality quick-drying water-based ink resin. The real-time monitoring of the viscosity sensor and the laser particle size analyzer can provide accurate data on the emulsion preparation state, which is crucial for the pre-emulsification control module. They help the control module make correct regulation decisions to ensure the uniformity and stability of the emulsion.

[0083] The pre-emulsification control module calculates the product of the first regulation information variable and the second regulation information variable to determine the regulation comparison value. There are a first standard regulation comparison value and a second standard regulation comparison value set in the pre-emulsification control module;

[0084] If the regulation comparison value is less than or equal to the first standard regulation comparison value, no regulation is performed on the pre-emulsification process;

[0085] If the regulation comparison value is greater than the first standard regulation comparison value and less than the second standard regulation comparison value, the pre-emulsification process is regulated by increasing the stirring speed;

[0086] If the regulation comparison value is greater than or equal to the second standard regulation comparison value, adjust the dropping speed of the mixed monomers.

[0087] Judging the pre-emulsification process comprehensively through viscosity data and particle size distribution uniformity ensures the accuracy of the judgment result. At the same time, by setting different intervals, different adjustments are made to the pre-emulsification to ensure the accuracy of the regulation. For those with small differences, no adjustment is made to maintain the stability of the pre-emulsification process. For those with medium differences, the rotation speed is adjusted to ensure that the pre-emulsification reaches the standard interval as soon as possible without destroying the ratio. For those with large differences, the reaction situation of the pre-emulsification is adjusted by adjusting the raw material addition speed so that it can fit the standard reaction as soon as possible.

[0088] For the process of pre - emulsification, the stirring speed is regulated to be increased, and the increased ratio is determined by the difference between the regulation ratio and the first standard regulation ratio.

[0089] For regulating the dropping speed of the mixed monomers, if the average value of the viscosity change curve F(1) is less than the average value of the viscosity change curve F(1), the dropping speed of the mixed monomers is increased; otherwise, it is decreased. The value for regulating the dropping speed of the mixed monomers is determined by the difference between the regulation ratio and the second standard regulation ratio.

[0090] Specifically, when the average value of the generated uniformity change curve is greater than or equal to the average value of the standard uniformity change curve, the pre - emulsification control module regulates the preparation process of the emulsification kettle only through the first regulation information variable.

[0091] Determining the regulation weight according to the data relationship between the first regulation information variable (viscosity) and the second regulation information variable (particle size) can achieve more refined control of the preparation process, optimize the preparation conditions of the emulsion, and improve the product quality. When the average value of the uniformity change curve is greater than or equal to the average value of the standard uniformity change curve, the pre - emulsification control module regulates only through viscosity, which can reduce unnecessary regulation actions, improve the preparation efficiency, and ensure the uniformity and stability of the emulsion at the same time.

[0092] Specifically, the dosage of the polymerization initiator solution is 0.8% of the total mass of the monomers, and ammonium persulfate prepared into a 10% aqueous solution.

[0093] Specifically, during the polymerization reaction, first pump 1 / 3 of the pre - emulsion into the reaction kettle, add the initiator solution, heat the reaction kettle to 70 °C, and adjust the stirring speed to 900 r / min. Maintain this temperature to initiate polymerization for 30 minutes, during which the blue light appears initially. Subsequently, the remaining pre - emulsion and the initiator solution are dropped synchronously according to the set curve to ensure a stable reaction at 75 - 80 °C for 2.5 hours, and the polymerization ends when the conversion rate monitored by near - infrared spectroscopy exceeds 90%.

[0094] Specifically, after the polymerization is completed, adjust the stirring speed to 700 r / min, adjust the temperature to 60 °C, add aziridine cross - linker, and introduce ammonia gas to maintain the pH value at 7 - 8 for cross - linking reaction.

[0095] Specifically, after cross - linking, cool to room temperature (25 °C), and the system automatically drops ammonia water precisely for neutralization according to the pH feedback; the product is automatically filtered through a 200 - mesh stainless - steel filter screen, and an alarm is given to prompt equipment maintenance when the amount of filter residue exceeds the threshold; the finished emulsion is pumped into the storage tank, and the liquid level, temperature, and nitrogen - protection atmosphere in the tank are all monitored intelligently. The solid content is determined by the automatic sampling and drying method to be 42% - 48%, and the stability exceeds 30 days without precipitation and stratification, ensuring that the resin can be supplied to downstream for formulating high - quality fast - drying water - based ink at any time.

[0096] So far, the technical solution of the present invention has been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easily understood by those skilled in the art that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

[0097] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a quick-drying water-based ink resin, characterized in that: include, The pre-emulsification control module drives each emulsification raw material storage device according to the preset ratio, injects the pre-emulsification raw materials into the emulsification kettle in a certain order, and controls the pre-emulsification process in real time to prepare the pre-emulsion; The polymerization control module adds part of the pre-emulsion and the polymerization initiator solution into the polymerization reactor. When the polymerization reaction reaches a certain degree, the remaining pre-emulsion and the polymerization initiator solution are added simultaneously according to a certain ratio. The polymerization is terminated after the conversion rate reaches the standard through real-time monitoring of the near infrared spectrum. Adding a cross-linking agent to the mixture after the polymerization is completed to prepare a crude resin; The prepared crude resin was cooled to room temperature and pH neutralized, and the product was filtered and stored; Real-time control of the pre-emulsification process includes: The pre-made mixed monomers are gradually added to the emulsion matrix. The viscosity sensor detects data to quantify the change in pre-emulsification viscosity; The uniformity of particle size distribution during the pre-emulsification process is determined by the detection data of the laser particle size analyzer; The viscosity change and particle size distribution uniformity were quantitatively processed together, and the stirring speed of the emulsifier and the rate of adding mixed monomers were re-determined.

2. The method for preparing the quick-drying water-based ink resin according to claim 1, characterized in that: The order of adding pre-emulsified raw materials into the emulsifying kettle is: Adding a nonionic emulsifier, octylphenol polyoxyethylene ether, and an anionic emulsifier, sodium lauryl sulfate, in a mass ratio of 1:1 and a total amount of 2.5% of the total mass of the monomers into deionized water, and starting a stirring device for stirring to prepare an emulsion matrix; After the stirring equipment runs smoothly, methyl methacrylate, butyl acrylate and hydroxyethyl acrylate are prepared into a mixed monomer in a mass ratio of 3:2:1, and are dripped into the emulsification kettle at a preset speed by a peristaltic pump; During the dropwise addition of the mixed monomers, online monitoring is performed by a viscosity sensor and a laser particle size analyzer, and the dropwise addition speed of the peristaltic pump is regulated according to the monitoring results.

3. The method for preparing the quick-drying water-based ink resin according to claim 2, characterized in that: The pre-emulsification control module determines a first control information variable according to data collected by the viscosity sensor, and determines a second control information variable according to data collected by the laser particle size analyzer. The pre-emulsification control module controls the preparation process of the emulsification kettle through the first control information variable and the second control information variable.

4. The method for preparing the quick-drying water-based ink resin according to claim 3, characterized in that: The viscosity sensor monitors the viscosity of the mixed solution in the emulsification kettle in real time, and transmits the monitoring result to the pre-emulsification control module, the pre-emulsification control module generates a viscosity change curve according to the monitored data, a standard viscosity change curve is arranged in the pre-emulsification control module, and the pre-emulsification control module determines the first control information variable according to the relationship between the generated viscosity change curve and the standard viscosity change curve.

5. The method for preparing the quick-drying water-based ink resin according to claim 3, characterized in that: The laser particle size analyzer monitors the distribution uniformity of the mixed solution in the emulsification kettle in real time, and transmits the monitoring result to the pre-emulsification control module, and the pre-emulsification control module generates a distribution uniformity change curve according to the monitored data. A standard distribution uniformity change curve is provided in the pre-emulsification control module, and the pre-emulsification control module determines the second control information variable according to the relationship between the generated distribution uniformity change curve and the standard distribution uniformity change curve.

6. The method for preparing the quick-drying water-based ink resin according to claim 3, characterized in that: The first control information variable is determined by comprehensive evaluation of the viscosity change dispersion, the viscosity change slope and the viscosity average value.

7. The method for preparing the quick-drying water-based ink resin according to claim 5, characterized in that: When the average value of the generated distribution uniformity change curve is greater than or equal to the average value of the standard distribution uniformity change curve, the pre-emulsification control module regulates the preparation process of the emulsification kettle only through the first regulation information variable.

8. The method for preparing the quick-drying water-based ink resin according to claim 1, characterized in that: The polymerization initiator solution is used in an amount of 0.8% of the total weight of the monomers, and is prepared as a 10% aqueous solution of ammonium persulfate.

9. The method for preparing the quick-drying water-based ink resin according to claim 8, characterized in that: During the polymerization reaction, first pump 1 / 3 of the pre-emulsion into the reactor, add the initiator solution, heat the reactor to 70°C, and adjust the stirring speed to 900r / min. Maintain this temperature to initiate polymerization for 30 minutes, during which time blue light begins to appear. Subsequently, add the remaining pre-emulsion and the initiator solution synchronously according to the set curve to ensure a stable reaction temperature of 75-80°C for 2.5 hours. The polymerization is terminated when the conversion rate exceeds 90% as monitored in real time by near-infrared spectroscopy.

10. The method for preparing the quick-drying water-based ink resin according to claim 1, characterized in that: After the polymerization is completed, the stirring speed is adjusted to 700 r / min, the temperature is adjusted to 60° C., an aziridine cross-linking agent is added, and ammonia is introduced to maintain the pH value at 7-8 to carry out a cross-linking reaction.

Citation Information

Patent Citations

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