Method and device for determining specific surface area of white carbon black and electronic equipment

Abstract

The invention discloses a method and device for determining the specific surface area of white carbon black and electronic equipment. The method comprises the steps that the first specific surface area of first white carbon black in an unknown vulcanized rubber sample is obtained, the first white carbon black is obtained after white carbon black extraction is conducted on the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained after the first white carbon black is tested through specific surface area and porosity analysis; acquiring a preset relation curve for representing a relation between a test value and a true value of the specific surface area of the white carbon black in the known vulcanized rubber sample; the first specific surface area is matched with a preset relation curve, the target specific surface area of the first white carbon black is obtained, and the target specific surface area is the true value of the specific surface area of the first white carbon black in the unknown vulcanized rubber sample. The method solves the technical problem of poor identification efficiency of the specific surface area of the white carbon black due to the fact that the white carbon black extracted by high-temperature burning is directly used for testing the specific surface area in related technologies.

Description

Technical Field

[0001] The present application relates to the technical field of rubber testing, and in particular to a method, device and electronic equipment for determining the specific surface area of ​​white carbon black. Background Art

[0002] In the rubber industry, especially in the field of tire production, white carbon black, as a high-performance filler, has attracted much attention because it can significantly reduce the rolling resistance of tires while maintaining good anti-ice and anti-wet skid resistance. As the concepts of environmental protection and energy conservation become more and more popular, the development of green tires has become a trend in the global tire industry. The application of white carbon black in formulations has become common, and even comparable to carbon black in cost. The qualitative and quantitative analysis of white carbon black is a key link in the research and development of rubber formulations, and the qualitative and quantitative analysis mainly involves three aspects: additive analysis, rubber analysis, and filler analysis. The core of filler analysis is the identification and quantification of carbon black and white carbon black.

[0003] In the related art, white carbon black can be separated from vulcanized rubber through cracking, burning, pickling and other steps. However, this method has certain limitations. First, the entire recovery process takes a long time, about 6 hours, and the operation is complicated; secondly, although the cracking temperature (such as within 600°C) and the burning temperature (such as within 750°C) can be controlled within a certain range in the related art so that it will not destroy the microstructure of white carbon black, it is found in actual operation that when the cracking temperature exceeds 500°C, the specific surface area of ​​white carbon black will be significantly reduced. This means that directly using the specific surface area value of white carbon black after high-temperature treatment to infer its type will inevitably produce large errors.

[0004] In summary, the silica detection method in the relevant technology is not only time-consuming and labor-intensive, but also has shortcomings in the recovery of the specific surface area of ​​silica. In particular, the specific surface area test after high-temperature treatment cannot accurately infer the type of original silica, which directly affects the evaluation and selection of material properties by formulation researchers.

[0005] To address the above-mentioned problems, no effective solution has been proposed yet. Summary of the invention

[0006] The embodiments of the present application provide a method, device and electronic device for determining the specific surface area of ​​white carbon black, so as to at least solve the technical problem that the identification efficiency of the specific surface area of ​​white carbon black is poor due to the specific surface area test of white carbon black directly extracted by high-temperature burning in the related art.

[0007] According to one aspect of an embodiment of the present application, a method for determining a specific surface area of ​​white carbon black is provided, comprising: obtaining a first specific surface area of ​​a first white carbon black in an unknown vulcanized rubber sample, wherein the first white carbon black is white carbon black obtained by extracting white carbon black from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first white carbon black through specific surface area and porosity analysis; obtaining a preset relationship curve for representing a relationship between a test value and a true value of the specific surface area of ​​white carbon black in a known vulcanized rubber sample; matching the first specific surface area with the preset relationship curve to obtain a target specific surface area of ​​the first white carbon black, wherein the target specific surface area is the true value of the specific surface area of ​​the first white carbon black in the unknown vulcanized rubber sample.

[0008] Optionally, the preset relationship curve is determined by: obtaining a second specific surface area of ​​initial silica in a known vulcanized rubber; obtaining a third specific surface area of ​​a second silica in a known vulcanized rubber sample, wherein the second silica is silica obtained by extracting silica from the known vulcanized rubber sample, and the third specific surface area is a test value obtained by testing the second silica using a specific surface area and porosity analyzer; and determining the preset relationship curve based on the second specific surface area and the third specific surface area.

[0009] Optionally, the raw materials of the initial white carbon black are at least five, and the specific surface area of ​​the initial white carbon black is in the range of 100 to 300 m 2 / g.

[0010] Optionally, the first white carbon black is extracted by at least the following methods: carbonization operation, burning operation, acid washing operation and filtering and washing operation.

[0011] Optionally, the burning operation is performed in a tubular muffle furnace with oxygen as the atmosphere, the oxygen flow rate of the burning operation is 300 to 500 mL / min, and the burning time is 30 to 50 min.

[0012] Optionally, the pickling operation uses a nitric acid solution with a ratio of 1:1, and the pickling time of the pickling operation is 10 to 20 minutes.

[0013] Optionally, the filtering and washing operation includes: filtering the filtrate of the unknown vulcanized rubber sample and the nitric acid solution to neutrality; and drying the filter residue of the unknown vulcanized rubber sample and the nitric acid solution to obtain the first white carbon black.

[0014] According to another aspect of an embodiment of the present application, a device for determining a specific surface area of ​​white carbon black is provided, comprising: a first acquisition module for acquiring a first specific surface area of ​​a first white carbon black in an unknown vulcanized rubber sample, wherein the first white carbon black is white carbon black obtained by extracting white carbon black from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first white carbon black through specific surface area and porosity analysis; a second acquisition module for acquiring a preset relationship curve for representing a relationship between a test value and a true value of the specific surface area of ​​white carbon black in a known vulcanized rubber sample; and a matching module for matching the first specific surface area with the preset relationship curve to obtain a target specific surface area of ​​the first white carbon black, wherein the target specific surface area is the true value of the specific surface area of ​​the first white carbon black in the unknown vulcanized rubber sample.

[0015] According to another aspect of the embodiments of the present application, there is also provided an electronic device, including: a memory and a processor, wherein the memory is used to store program instructions; the processor is connected to the memory and is used to execute the above-mentioned method for determining the specific surface area of ​​white carbon black.

[0016] According to another aspect of the embodiments of the present application, a non-volatile storage medium is also provided, the non-volatile storage medium includes a stored computer program, wherein the device where the non-volatile storage medium is located executes the above-mentioned method for determining the specific surface area of ​​white carbon black by running the computer program.

[0017] According to another aspect of the embodiments of the present application, a computer program product is also provided, including computer instructions, which implement the above-mentioned method for determining the specific surface area of ​​white carbon black when the computer instructions are executed by a processor.

[0018] In an embodiment of the present application, a first specific surface area of ​​a first silica in an unknown vulcanized rubber sample is obtained, wherein the first silica is the silica obtained by extracting silica from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first silica through specific surface area and porosity analysis; a preset relationship curve is obtained to represent the relationship between the test value and the true value of the specific surface area of ​​silica in a known vulcanized rubber sample; the first specific surface area is matched with the preset relationship curve to obtain a target specific surface area of ​​the first silica, wherein the target specific surface area is the true value of the specific surface area of ​​the first silica in the unknown vulcanized rubber sample, thereby achieving the purpose of matching with the preset relationship curve to accurately identify the original specific surface area of ​​silica, thereby achieving the technical effect of improving the accuracy and efficiency of the identification of the specific surface area of ​​silica, and further solving the technical problem of poor identification efficiency of the specific surface area of ​​silica due to the direct use of silica extracted by high-temperature burning for specific surface area testing in the related art. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The drawings described herein are used to provide a further understanding of the present application and constitute a part of the present application. The illustrative embodiments of the present application and their descriptions are used to explain the present application and do not constitute an improper limitation on the present application. In the drawings:

[0020] Figure 1 is a hardware structure diagram of a computer terminal for implementing a method for determining the specific surface area of ​​white carbon black according to an embodiment of the present application;

[0021] Figure 2 is a flow chart of a method for determining the specific surface area of ​​white carbon black according to an embodiment of the present application;

[0022] Figure 3 is a schematic diagram of a preset relationship curve according to an embodiment of the present application;

[0023] Figure 4 It is a structural diagram of a device for determining the specific surface area of ​​white carbon black according to an embodiment of the present application. DETAILED DESCRIPTION

[0024] In order to enable those skilled in the art to better understand the solution of the present application, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present application.

[0025] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchangeable where appropriate, so that the embodiments of the present application described herein can be implemented in an order other than those illustrated or described herein. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0026] First, some nouns or terms that appear in the process of explaining the embodiments of the present application are subject to the following explanations:

[0027] White carbon black: In the rubber industry, white carbon black is a high-performance inorganic non-metallic material, the main component of which is silicon dioxide (SiO2). Compared with carbon black, white carbon black has higher dispersibility and lower rolling resistance, can improve the tire's anti-slip and wear resistance, and is an important formula component for green tires.

[0028] Specific surface area: A physical quantity that measures the surface area of ​​a substance per unit mass or unit volume. In rubber formulations, the specific surface area of ​​silica directly affects its dispersibility and reinforcement effect in the rubber matrix.

[0029] Fully automatic rapid specific surface area and porosity analyzer (Gemini VII 2390t): A high-performance analytical instrument used to quickly and accurately determine the specific surface area and porosity of materials. It uses BET theory and physical methods such as nitrogen adsorption to calculate the specific surface area parameters of the material.

[0030] BET (Brunauer-Emmett-Teller): A theory and method for measuring the specific surface area of ​​solid materials, proposed by three scientists, Stephen Brunauer, Edwin Emmett and Lynard Teller in 1938. The BET method is based on the multilayer adsorption theory and is suitable for measuring the adsorption characteristics of solid materials with large specific surface areas, and determines the total surface area of ​​the material by physical adsorption (usually gas adsorption, such as nitrogen, argon, etc.).

[0031] Muffle furnace: A laboratory equipment used for high temperature processing, which can perform operations such as sintering, melting, ashing, and heat treatment of samples. In the process of silica extraction, the muffle furnace is used to remove rubber and carbon black components under controlled temperature and atmosphere to recover silica.

[0032] Drying oven: A device used to dry samples. By controlling temperature and time, it can remove moisture from the sample and achieve sample drying, providing necessary pretreatment for the determination of the specific surface area of ​​silica.

[0033] In order to solve the problem of poor detection efficiency of white carbon black specific surface area in the related art, the present application embodiment provides a method for determining the specific surface area of ​​white carbon black, which can be run on Figure 1 In the computer terminal shown, the computer terminal is described below.

[0034] The method for determining the specific surface area of ​​white carbon black provided in the embodiments of the present application can be executed in a mobile terminal, a computer terminal or a similar computing device. Figure 1 The hardware structure block diagram of a computer terminal for implementing a method for determining the specific surface area of ​​white carbon black is shown. Figure 1As shown, the computer terminal 10 may include one or more (102a, 102b, ..., 102n are used to illustrate) processors (the processor may include but is not limited to a processing device such as a microprocessor MCU or a programmable logic device FPGA), a memory 104 for storing data, and a transmission module 106 for communication functions connected via a wired and / or wireless network. In addition, it may also include: a display, a keyboard, a cursor control device, an input / output interface (I / O interface), a universal serial bus (USB) port (which may be included as one of the ports of the I / O interface), a network interface, and a BUS bus. Those skilled in the art can understand that Figure 1 The structure shown is only for illustration and does not limit the structure of the above electronic device. Figure 1 More or fewer components as shown, or with Figure 1 Different configurations are shown.

[0035] It should be noted that the one or more processors and / or other data processing circuits described above may generally be referred to herein as "data processing circuits". The data processing circuits may be embodied in whole or in part as software, hardware, firmware, or any other combination thereof. In addition, the data processing circuit may be a single independent processing module, or may be incorporated in whole or in part into any of the other components in the computer terminal 10. As described in the embodiments of the present application, the data processing circuit acts as a processor control (e.g., selection of a variable resistor terminal path connected to an interface).

[0036] The memory 104 can be used to store software programs and modules of application software, such as the program instructions / data storage device corresponding to the method for determining the specific surface area of ​​white carbon black in the embodiment of the present application. The processor executes various functional applications and data processing by running the software programs and modules stored in the memory 104, that is, the above-mentioned method for determining the specific surface area of ​​white carbon black is realized. The memory 104 may include a high-speed random access memory, and may also include a non-volatile memory, such as one or more magnetic storage devices, flash memory, or other non-volatile solid-state memory. In some examples, the memory 104 may further include a memory remotely arranged relative to the processor, and these remote memories may be connected to the computer terminal 10 via a network. Examples of the above-mentioned network include, but are not limited to, the Internet, an intranet, a local area network, a mobile communication network, and combinations thereof.

[0037] The transmission module 106 is used to receive or send data via a network. The specific example of the above network may include a wireless network provided by a communication provider of the computer terminal 10. In one example, the transmission module 106 includes a network adapter (Network Interface Controller, NIC), which can be connected to other network devices through a base station so as to communicate with the Internet. In one example, the transmission module 106 can be a radio frequency (RF) module, which is used to communicate with the Internet wirelessly.

[0038] The display may be, for example, a touch screen liquid crystal display (LCD) that enables a user to interact with a user interface of the computer terminal 10 .

[0039] It should be noted that, in some optional embodiments, the above Figure 1 The computer terminal shown may include hardware elements (including circuits), software elements (including computer code stored on a computer-readable medium), or a combination of hardware elements and software elements. It should be noted that Figure 1 This is merely one example of a particular embodiment and is intended to illustrate the types of components that may be present in the computer terminal described above.

[0040] Under the above operating environment, an embodiment of the present application provides an embodiment of a method for determining the specific surface area of ​​white carbon black. It should be noted that the steps shown in the flowchart of the accompanying drawings can be executed in a computer system such as a set of computer executable instructions, and although the logical order is shown in the flowchart, in some cases, the steps shown or described can be executed in an order different from that shown here.

[0041] Figure 2 is a flow chart of a method for determining the specific surface area of ​​white carbon black according to an embodiment of the present application, such as Figure 2 As shown, the method comprises the following steps:

[0042] Step S202, obtaining a first specific surface area of ​​a first silica in the unknown vulcanized rubber sample, wherein the first silica is silica obtained by extracting silica from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first silica through specific surface area and porosity analysis.

[0043] In the above step S202, it is first necessary to process an unknown vulcanized rubber sample, which may come from a tire or other rubber product, containing white carbon black of unknown type and specific surface area. Subsequently, the unknown vulcanized rubber sample is sheared into small particles, and the rubber, carbon black and other non-white carbon black components are removed through steps such as carbonization, burning, pickling, filtering, washing and drying, so as to purify and recover the white carbon black, that is, the first white carbon black mentioned above. These steps ensure the purity of the first white carbon black finally obtained, making it suitable for subsequent specific surface area tests. It should be noted that the key to the carbonization and burning process lies in the control of temperature and time to minimize the impact on the microstructure of white carbon black, because in actual operation, a temperature exceeding 500°C will cause a significant reduction in the specific surface area of ​​white carbon black.

[0044] Furthermore, the first white carbon black after extraction is tested by a fully automatic rapid specific surface area and porosity analyzer (such as Gemini VII 2390t) to obtain the first specific surface area of ​​the first white carbon black. This instrument uses the BET method to measure the specific surface area of ​​the material, which is highly accurate and easy to operate. During the test, high-purity nitrogen (purity above 99.9%) can be used as the adsorption gas, and liquid nitrogen (purity above 99.8%) can be used as the cooling medium to provide a low-temperature environment to ensure that the gas molecules can be effectively adsorbed to the solid surface. At the same time, different relative pressure P / P0 selection points (0.05, 0.06, 0.07, 0.075, 0.08, 0.09, 0.10) can also be set to obtain more comprehensive adsorption data, thereby accurately determining the specific surface area of ​​the material.

[0045] Step S204, obtaining a preset relationship curve for representing the relationship between the test value and the true value of the specific surface area of ​​white carbon black in the known vulcanized rubber sample.

[0046] In the above step S204, the preset relationship curve is established by extracting and testing a series of white carbon black samples with known specific surface areas to establish a mathematical relationship between the specific surface area (test value) of the white carbon black after high temperature treatment and the original specific surface area (true value).

[0047] like Figure 3 As shown, in this application, five kinds of white carbon black with different specific surface areas are used as experimental materials. The preset relationship curve between the specific surface area x obtained after the extraction step in step S202 and its original specific surface area y is y=1.2026x+12.276, where R 2 =0.9964, indicating a good fit of the preset relationship curve.

[0048] The importance of establishing a preset relationship curve is that it can correct the effect of high temperature treatment (such as carbonization and burning) on ​​the specific surface area of ​​silica. In actual operation, temperatures exceeding 500°C will cause a significant decrease in the specific surface area of ​​silica, which directly means that directly using recycled silica for specific surface area testing will result in a lower value. The preset relationship curve can convert the test value into a true value that is closer to the original state, thereby improving the accuracy of identifying the type and specific surface area of ​​silica in unknown vulcanized rubber samples. Through this preset relationship curve, when the test value of the unknown sample is subsequently converted, a relatively accurate specific surface area can be obtained, providing reliable data support for rubber formula design and product quality control.

[0049] Step S206, matching the first specific surface area with a preset relationship curve to obtain a target specific surface area of ​​the first white carbon black, wherein the target specific surface area is a true value of the specific surface area of ​​the first white carbon black in the unknown vulcanized rubber sample.

[0050] In the above step S206, the first specific surface area obtained in step S202 is substituted into the preset relationship curve y=1.2026x+12.276 established in step S204, and mathematical operations are performed to directly calculate the target specific surface area of ​​the first silica, that is, the actual specific surface area of ​​silica in the unknown vulcanized rubber sample.

[0051] Through the above steps S202 to S206, the purpose of matching with the preset relationship curve to accurately identify the original specific surface area of ​​white carbon is achieved, thereby achieving the technical effect of improving the accuracy and efficiency of the identification of the specific surface area of ​​white carbon, and further solving the technical problem that the identification efficiency of the specific surface area of ​​white carbon is poor due to the specific surface area test of white carbon directly extracted by high-temperature burning in the related art. The following is a detailed description.

[0052] In the above step S204, the preset relationship curve is determined by the following method: obtaining a second specific surface area of ​​initial silica in a known vulcanized rubber; obtaining a third specific surface area of ​​a second silica in a known vulcanized rubber sample, wherein the second silica is silica obtained by extracting silica from the known vulcanized rubber sample, and the third specific surface area is a test value obtained by testing the second silica using a specific surface area and porosity analyzer; and determining the preset relationship curve based on the second specific surface area and the third specific surface area.

[0053] Furthermore, the raw materials of the initial white carbon black are at least five, and the specific surface area of ​​the initial white carbon black is in the range of 100 to 300 m 2 / g.

[0054] In the embodiment of the present application, the method for determining the preset relationship curve is a statistical analysis method based on experimental data, which is used to calibrate and predict the true specific surface area of ​​white carbon black in an unknown vulcanized rubber sample. The specific process can be as follows:

[0055] First, at least five initial silica samples were selected. The raw material differences of these samples ensured the comprehensiveness and representativeness of the data. In particular, the specific surface area range of these silica samples was limited to 100-300 m 2 / g, which is a relatively broad but targeted range that can cover the specific surface area variation range of silica in most vulcanized rubber formulations, ensuring the applicability and predictive ability of the preset relationship curve.

[0056] Secondly, for each initial silica, use a specific surface area and porosity analyzer (such as Gemini VII2390t) under standard test conditions to measure its original specific surface area to obtain a second specific surface area. In the present embodiment, the test values ​​y of the specific surface areas of the five initial silicas are: 127 m 2 / g, 149m 2 / g, 161m 2 / g, 183m 2 / g, 205m 2 / g. These data reflect the real physical properties of silica before adding it to the vulcanized rubber and are the basis for constructing the preset relationship curve.

[0057] Next, for the known vulcanized rubber sample containing the above-mentioned initial silica, a series of extraction and processing steps are performed, including carbonization, burning, pickling, filtering and drying, to separate and purify the silica from the vulcanized rubber to obtain a second silica. Then, the treated second silica is tested using the same specific surface area and porosity analyzer to obtain a third specific surface area. In the embodiment of the present application, the test values ​​x of the specific surface area of ​​the extracted second silica are: 94m 2 / g, 114m 2 / g, 126m 2 / g, 142m 2 / g, 159m 2 / g. This data point reflects the change in the specific surface area of ​​silica after high temperature treatment and is an important indicator for evaluating the effect of high temperature treatment on the properties of silica.

[0058] Further, the second specific surface area of ​​each initial silica is paired with the third specific surface area of ​​the corresponding second silica after treatment to form (x, y) data points. Where x represents the third specific surface area and y represents the second specific surface area. Statistical methods, such as linear regression analysis, are used to fit these data points to determine the relationship y=kx+b, where k represents the slope and b represents the intercept. The purpose is to establish a mathematical model that can accurately predict the relationship between the specific surface area test value of silica after high temperature treatment and the original specific surface area in any unknown vulcanized rubber sample. The specific steps can be as follows:

[0059] Step 1: First, ensure that all (x, y) data points are complete and free of outliers through data preprocessing. For example, when the dimensions or ranges of the original data vary greatly, data standardization (such as normalizing the specific surface area value) is required to eliminate the dimensional effect and improve the efficiency and stability of model training.

[0060] Step 2: Use linear regression analysis, based on the principle of minimizing the sum of squares of prediction errors, to determine the optimal slope k and intercept b through iterative calculation to establish the relationship y=kx+b.

[0061] Step 3: The model can be evaluated by calculating R 2 The coefficient of determination and residual analysis are implemented. For example, R 2 Evaluate the model's fit, which reflects the proportion of the variation explained by the model to the total variation. An R close to 1 2 A value of 0 indicates that the model has good predictive ability. Alternatively, check whether the differences between the model predictions and the actual values ​​(residuals) are randomly distributed to ensure that the model has no systematic bias. If the data points in the residual plot are evenly distributed around 0, it means that the model predicts well.

[0062] Finally, after the preset relationship curve is initially determined, additional known vulcanized rubber samples can be tested to verify the accuracy and reliability of the curve. The specific steps can be as follows:

[0063] Step 1: Select a set of additional known vulcanized rubber samples, where the actual specific surface area of ​​silica in these additional samples should cover the entire target specific surface area range to ensure the comprehensiveness of the model.

[0064] Step 2: For each additional sample, calculate the difference between its true specific surface area and the model predicted value to obtain the prediction error, and visually observe the distribution of the error by drawing an error histogram or scatter plot.

[0065] If the prediction error is found to increase significantly over a certain range of surface area, or if a particular type of silica is predicted inaccurately, this may indicate that the model needs to be adjusted to accommodate a wider range of data under these conditions.

[0066] Step 3: Based on error analysis, fine-tune the parameters of the linear regression model (slope k and intercept b) to find the best parameter combination to reduce the prediction error. In order to improve the robustness and accuracy of the model, you can also add data points in areas with large deviations and retrain the model with more extensive experimental data to better fit the actual change trend.

[0067] Step 4: Use the adjusted preset relationship curve to predict another group of independent known vulcanized rubber samples to verify the accuracy and generalization ability of the model again. By calculating the accuracy and stability of the adjusted model prediction, such as the new R 2 The value, mean square error (MSE), etc. are used to evaluate whether the overall performance of the model has been improved. If the adjusted model performs well on the new validation data and the prediction results are stable in the entire specific surface area range, the applicability of the preset relationship curve can be confirmed, providing a reliable benchmark for predicting the specific surface area of ​​silica in unknown vulcanized rubber samples.

[0068] Through the above process, the preset relationship curve constructed can not only reflect the change law of the specific surface area of ​​white carbon black during the vulcanized rubber treatment process, but also provide a quantitative method to accurately predict the true specific surface area of ​​white carbon black in unknown vulcanized rubber samples, which is of great significance to rubber formulation research and quality control. The construction of the preset relationship curve is based on carefully designed experimental data and rigorous statistical analysis, ensuring that in the subsequent step S206, when the first specific surface area is matched with the curve, a reliable target specific surface area of ​​the first white carbon black can be obtained.

[0069] In the above steps, the first white carbon black is extracted by at least the following methods: carbonization operation, burning operation, acid washing operation and filtering and washing operation.

[0070] In the examples of the present application, both the first silica (silica in an unknown vulcanized rubber sample) and the second silica (silica in a known vulcanized rubber sample used to establish a relationship curve) have their extraction and identification processes follow a set of standardized steps, including carbonization, burning, pickling, and filtering and washing operations, with the goal of separating, purifying, and identifying the specific surface area of ​​silica from a complex vulcanized rubber matrix.

[0071] The entire extraction and identification process is designed to reduce the impact of high-temperature treatment on the structure of silica, and accurately correct the change in specific surface area by establishing a relationship curve, thereby providing accurate data support for formulation researchers and facilitating the research and development and quality control of rubber products such as tires.

[0072] Among them, carbonization is the starting step of the extraction process, and its role is to remove the organic components in the vulcanized rubber, including rubber and additives. The sample is cut into small pieces and placed in a porcelain crucible or a quartz crucible, and heated on an adjustable electric furnace or hot plate until it turns gray (indicating that the organic matter has been carbonized). These crucibles are resistant to high temperatures and have stable chemical properties. They will not react with the vulcanized rubber or white carbon black, ensuring the purity and integrity of the sample. At the same time, the carbonization temperature should be controlled below 600°C, and in actual operation should not exceed 500°C, so as to maintain the integrity of the white carbon black structure as much as possible and avoid a significant reduction in its specific surface area.

[0073] Optionally, the burning operation is performed in a tubular muffle furnace with oxygen as the atmosphere, the oxygen flow rate of the burning operation is 300 to 500 mL / min, and the burning time is 30 to 50 min.

[0074] In the embodiment of the present application, the burning operation is performed in a tubular muffle furnace in an oxygen atmosphere. By controlling the oxygen flow rate and the burning time, the organic impurities in the vulcanized rubber sample can be effectively removed, and the white carbon black can be purified and recovered. This operation not only ensures efficiency, but also pays attention to the protection of the properties of white carbon black, providing a pure sample for subsequent specific surface area testing and identification.

[0075] Among them, the tubular muffle furnace is a high-temperature heating equipment suitable for heat treatment of samples under a specific atmosphere. The tubular design of the muffle furnace allows oxygen to contact the sample evenly, ensuring that the structure and properties of white carbon black can still be accurately tested and identified after high-temperature treatment. Oxygen is a strong oxidant. Placing the sample in an oxygen atmosphere for burning accelerates the oxidation process of organic matter, which can ensure that the organic matter in the vulcanized rubber (such as rubber and carbon black) can be completely oxidized and decomposed, and help to obtain pure white carbon black in a shorter time. The oxygen flow rate is set in the range of 300-500mL / min. This parameter is selected to ensure that while ensuring sufficient oxygen supply, avoid unnecessary waste or excessive reaction caused by excessive flow. Appropriate oxygen flow ensures that the sample can be evenly exposed to oxygen, promotes the complete oxidation of organic matter, and also helps to control the atmosphere in the furnace to avoid overoxidation or other side reactions. The burning time is set at 30-50min. This time interval is determined based on experimental optimization, aiming to ensure that the organic matter in the sample is completely oxidized, while avoiding the damage to the structure of white carbon black caused by excessively long high-temperature treatment.

[0076] Optionally, the pickling operation uses a nitric acid solution with a ratio of 1:1, and the pickling time of the pickling operation is 10 to 20 minutes.

[0077] In the examples of this application, the pickling operation dissolves inorganic impurities to prepare a pure sample for the subsequent specific surface area test. Correct acid selection, concentration control, time setting, and subsequent safety and environmental protection treatment are all key factors to ensure the accuracy of silica properties and experimental results.

[0078] For example, a nitric acid solution with a ratio of 1:1 can be used for pickling. Nitric acid is a strongly oxidizing and strongly acidic inorganic acid that can effectively dissolve metal oxides, such as zinc oxide (ZnO) and calcium carbonate (CaCO3). These ingredients are common in vulcanized rubber formulations, but they are interference factors in the specific surface area test of white carbon black. Using nitric acid as a pickling agent can remove these impurities in a targeted manner without destroying the structure of white carbon black. At the same time, the 1:1 ratio and concentration provide a sufficient acidic environment to dissolve metal oxides, while also avoiding the damage that may be caused to white carbon black or experimental equipment by using an overly concentrated acid solution. The pickling time can be set at 10 to 20 minutes. This time window is the result of experimental optimization, which aims to ensure that impurities are fully dissolved while avoiding the potential damage to the structure of white carbon black by long-term pickling. Too short a time may not completely remove impurities, while too long a time may cause unnecessary side reactions or structural changes in white carbon black, affecting the accuracy of subsequent specific surface area tests.

[0079] In general, the pickling operation is usually carried out after the sample has been carbonized and burned, and the organic matter and most of the carbon black have been removed. The burned sample is ground into a powder, then added to a nitric acid solution and heated and soaked for 10 to 20 minutes. The purpose of heating is to speed up the chemical reaction rate and ensure that impurities can be quickly dissolved by nitric acid. Subsequently, through subsequent steps such as filtration and washing, the acid and other impurities are further removed to obtain pure white carbon black.

[0080] Optionally, the filtering and washing operation includes: filtering the filtrate of the unknown vulcanized rubber sample and the nitric acid solution to neutrality; and drying the filter residue of the unknown vulcanized rubber sample and the nitric acid solution to obtain the first white carbon black.

[0081] In the embodiments of the present application, the filtering and washing operation is the last step in the extraction and purification process of silica, and its purpose is to further remove the acid solution and other impurities remaining after pickling, to ensure that the final silica sample is pure and suitable for accurate testing of specific surface area.

[0082] Due to the soaking and preliminary filtration during the pickling process, acid and dissolved metal ions may still remain in the filtrate. Therefore, the filtrate needs to be filtered to neutrality, for example, by multiple washings and filtering with neutral liquids such as distilled water to neutralize the residual acidic substances until the pH value of the filtrate is close to 7, that is, neutral, to remove the dissolved metal ions and avoid these impurities from re-precipitating on the silica in subsequent steps, affecting its purity and the reliability of the test. The filter residue after pickling and filtration, that is, the solid substance mainly composed of silica, needs to be dried to obtain the final pure silica sample. During the drying process, the sample is usually placed in a drying oven to evaporate the residual water and solution at a suitable temperature.

[0083] Through the two steps of filtering to neutrality and drying, not only the acid and impurities remaining after pickling are removed, but also the dryness and purity of the first and second white carbon blacks are ensured, providing high-quality samples for subsequent specific surface area tests. It should be noted that in actual operation, the filtering and washing operations need to be repeated many times until the washed filtrate reaches neutrality and the weight of the filter residue does not change after drying, so that the extracted white carbon black reaches the ideal purity.

[0084] In order to clearly demonstrate the practical application effect of the method for determining the specific surface area of ​​white carbon in the vulcanized rubber in the embodiments of the present application, three examples are listed below for illustration.

[0085] Example 1: A tread vulcanized rubber is provided, and 200MP of white carbon black is added. First, the white carbon black in the vulcanized rubber is extracted. The extraction process is as described above. The specific surface area of ​​the extracted and recovered white carbon black is 170m 2 / g, and put it into the relationship curve y = 1.2026x + 12.276, the specific surface area of ​​the raw material white carbon black is calculated to be 217m 2 / g, thus inferring that the raw material white carbon black is 200MP, which is consistent with the actual formula.

[0086] Example 2: A tread vulcanized rubber is provided, and 7000GR of white carbon black is added. First, the white carbon black in the vulcanized rubber is extracted. The extraction process is as described above. The specific surface area of ​​the extracted and recovered white carbon black is 136m 2 / g, and put it into the relationship curve y = 1.2026x + 12.276, the specific surface area of ​​the raw material white carbon black is calculated to be 176m 2 / g, thus inferring that the raw material white carbon black is 7000GR, which is consistent with the actual formula.

[0087] Example 3: A tread vulcanized rubber is provided, and the added white carbon black is 1125MP. First, the white carbon black in the vulcanized rubber is extracted. The extraction process is as described above. The specific surface area of ​​the extracted white carbon black is 96m 2 / g, and put it into the relationship curve y = 1.2026x + 12.276, the specific surface area of ​​the raw material white carbon black is calculated to be 128m 2 / g, thus inferring that the raw material white carbon black is 1125MP, which is consistent with the actual formula.

[0088] In the examples of the present application, by establishing a relationship curve between the specific surface area test value of the burned recovered white carbon black and the specific surface area value of the original white carbon black, the error problem existing when directly using the specific surface area test value of the burned white carbon black to infer the type of white carbon black is solved. At the same time, by optimizing the operating conditions such as carbonization, burning, pickling, filtering and washing, the microstructure of white carbon black is effectively protected, the significant effect of high temperature treatment on the specific surface area of ​​white carbon black is avoided, and the accuracy and efficiency of identification are improved. Its beneficial effects are significant, and it can provide more accurate data support for rubber formulation research, especially in the green manufacturing and performance optimization of products such as tires. It has important application potential, and promotes the scientific and technological progress of the rubber industry and the realization of environmental protection and energy-saving goals.

[0089] According to an embodiment of the present application, a device for determining the specific surface area of ​​white carbon black is provided. It should be noted that the device for determining the specific surface area of ​​white carbon black in the embodiment of the present application can be used to execute the method for determining the specific surface area of ​​white carbon black provided in the embodiment of the present application. The device for determining the specific surface area of ​​white carbon black provided in the embodiment of the present application is introduced below.

[0090] Figure 4 1 is a structural diagram of a device for determining the specific surface area of ​​white carbon black provided in an embodiment of the present application. Figure 4 As shown, the device comprises:

[0091] A first acquisition module 40 is used to obtain a first specific surface area of ​​a first white carbon black in an unknown vulcanized rubber sample, wherein the first white carbon black is white carbon black obtained by extracting white carbon black from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first white carbon black through specific surface area and porosity analysis;

[0092] A second acquisition module 42 is used to acquire a preset relationship curve for representing the relationship between a test value and a true value of a known specific surface area of ​​white carbon black in a vulcanized rubber sample;

[0093] The matching module 44 is used to match the first specific surface area with a preset relationship curve to obtain a target specific surface area of ​​the first white carbon black, wherein the target specific surface area is a true value of the specific surface area of ​​the first white carbon black in the unknown vulcanized rubber sample.

[0094] Through the first acquisition module 40, the second acquisition module 42 and the matching module 44 in the above-mentioned device for determining the specific surface area of ​​white carbon, the purpose of matching in combination with the preset relationship curve to accurately identify the original specific surface area of ​​white carbon is achieved, thereby achieving the technical effect of improving the accuracy and efficiency of the identification of the specific surface area of ​​white carbon, and further solving the technical problem of poor identification efficiency of the specific surface area of ​​white carbon due to the direct use of white carbon extracted by high-temperature burning for specific surface area testing in the related technology.

[0095] An embodiment of the present application also provides an electronic device, including: a memory and a processor, wherein the memory is used to store program instructions; the processor is connected to the memory and is used to execute the above-mentioned method for determining the specific surface area of ​​white carbon black.

[0096] It should be noted that the above electronic equipment is used to execute Figure 2 The method for determining the specific surface area of ​​white carbon black is shown in the figure, so the relevant explanations in the above method for determining the specific surface area of ​​white carbon black are also applicable to the electronic device and will not be repeated here.

[0097] An embodiment of the present application also provides a non-volatile storage medium, which includes a stored computer program, wherein the device where the non-volatile storage medium is located executes the above-mentioned method for determining the specific surface area of ​​white carbon black by running the computer program.

[0098] It should be noted that the above non-volatile storage medium is used to execute Figure 2 The method for determining the specific surface area of ​​white carbon black is shown in the figure, so the relevant explanations in the above method for determining the specific surface area of ​​white carbon black are also applicable to the non-volatile storage medium, and will not be repeated here.

[0099] An embodiment of the present application also provides a computer program product, including computer instructions, which, when executed by a processor, implement the above-mentioned method for determining the specific surface area of ​​white carbon black.

[0100] It should be noted that the above-mentioned computer program product is used to execute Figure 2 The method for determining the specific surface area of ​​white carbon black is shown in the figure, so the relevant explanations in the above method for determining the specific surface area of ​​white carbon black are also applicable to the computer program product and will not be repeated here.

[0101] The serial numbers of the above-mentioned embodiments of the present application are for description only and do not represent the advantages or disadvantages of the embodiments.

[0102] In the above embodiments of the present application, the description of each embodiment has its own emphasis. For parts that are not described in detail in a certain embodiment, please refer to the relevant description of other embodiments.

[0103] In the several embodiments provided in this application, it should be understood that the disclosed technical content can be implemented in other ways. Among them, the device embodiments described above are only schematic. For example, the division of the units can be a logical function division. There may be other division methods in actual implementation. For example, multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed. Another point is that the mutual coupling or direct coupling or communication connection shown or discussed can be through some interfaces, indirect coupling or communication connection of units or modules, which can be electrical or other forms.

[0104] The units described as separate components may or may not be physically separated, and the components shown as units may or may not be physical units, that is, they may be located in one place or distributed on multiple units. Some or all of the units may be selected according to actual needs to achieve the purpose of the present embodiment.

[0105] In addition, each functional unit in each embodiment of the present application may be integrated into one processing unit, or each unit may exist physically separately, or two or more units may be integrated into one unit. The above-mentioned integrated unit may be implemented in the form of hardware or in the form of software functional units.

[0106] If the integrated unit is implemented in the form of a software functional unit and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present application, in essence, or the part that contributes to the prior art or all or part of the technical solution can be embodied in the form of a software product, and the computer software product is stored in a storage medium, including a number of instructions to enable a computer device (which can be a personal computer, a server or a network device, etc.) to perform all or part of the steps of the method described in each embodiment of the present application. The aforementioned storage medium includes: U disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), mobile hard disk, disk or optical disk and other media that can store program codes.

[0107] The above is only a preferred implementation of the present application. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present application. These improvements and modifications should also be regarded as the scope of protection of the present application.

Claims

1. A method for determining the specific surface area of ​​white carbon black, characterized in that: include: Obtaining a first specific surface area of ​​a first white carbon black in an unknown vulcanized rubber sample, wherein the first white carbon black is white carbon black obtained by extracting white carbon black from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first white carbon black through specific surface area and porosity analysis; Obtaining a preset relationship curve for representing the relationship between a test value and a true value of a known specific surface area of ​​white carbon black in a vulcanized rubber sample; The first specific surface area is matched with the preset relationship curve to obtain a target specific surface area of ​​the first white carbon black, wherein the target specific surface area is a true value of the specific surface area of ​​the first white carbon black in the unknown vulcanized rubber sample.

2. The method according to claim 1, characterized in that The preset relationship curve is determined by: Obtaining a second specific surface area of ​​initial silica in the known vulcanized rubber; Obtaining a third specific surface area of ​​a second white carbon black in the known vulcanized rubber sample, wherein the second white carbon black is white carbon black obtained by extracting white carbon black from the known vulcanized rubber sample, and the third specific surface area is a test value obtained by testing the second white carbon black using the specific surface area and porosity analyzer; The preset relationship curve is determined according to the second specific surface area and the third specific surface area.

3. The method according to claim 2, characterized in that The raw materials of the initial white carbon black are at least five, and the specific surface area of ​​the initial white carbon black is in the range of 100 to 300 m 2 / g.

4. The method according to claim 1, characterized in that: The first white carbon black is extracted by at least the following methods: carbonization operation, burning operation, pickling operation and filtering and washing operation.

5. The method according to claim 4, characterized in that The burning operation is carried out in a tubular muffle furnace with oxygen as the atmosphere, the oxygen flow rate of the burning operation is 300-500 mL / min, and the burning time is 30-50 min.

6. The method according to claim 4, characterized in that The pickling operation uses a nitric acid solution with a ratio of 1:1, and the pickling time of the pickling operation is 10 to 20 minutes.

7. The method according to claim 6, characterized in that The filtering and washing operation includes: filtering the filtrate of the unknown vulcanized rubber sample and the nitric acid solution to neutrality; and drying the filter residue of the unknown vulcanized rubber sample and the nitric acid solution to obtain the first white carbon black.

8. A device for determining the specific surface area of ​​white carbon black, characterized in that: include: A first acquisition module is used to obtain a first specific surface area of ​​a first white carbon black in an unknown vulcanized rubber sample, wherein the first white carbon black is white carbon black obtained by extracting white carbon black from the unknown vulcanized rubber sample, and the first specific surface area is a test value obtained by testing the first white carbon black through specific surface area and porosity analysis; A second acquisition module is used to acquire a preset relationship curve for representing the relationship between a test value and a true value of a known specific surface area of ​​white carbon black in a vulcanized rubber sample; A matching module is used to match the first specific surface area with the preset relationship curve to obtain a target specific surface area of ​​the first white carbon black, wherein the target specific surface area is a true value of the specific surface area of ​​the first white carbon black in the unknown vulcanized rubber sample.

9. An electronic device, characterized in that: include: A memory and a processor, wherein the memory is used to store program instructions; The processor is connected to the memory and is used to execute the method for determining the specific surface area of ​​white carbon black as described in any one of claims 1 to 7.

10. A non-volatile storage medium, characterized in that: The non-volatile storage medium includes a stored computer program, wherein the device where the non-volatile storage medium is located executes the method for determining the specific surface area of ​​white carbon black according to any one of claims 1 to 7 by running the computer program.

11. A computer program product comprising computer instructions, characterized in that: When the computer instructions are executed by a processor, the method for determining the specific surface area of ​​white carbon black according to any one of claims 1 to 7 is implemented.

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