A method for rapid detection of properties of silica-containing rubber, applications and computer program product

One-stop testing using RPA solves the problem that traditional testing methods cannot quickly detect the performance of vulcanized rubber, enabling comprehensive testing of both unvulcanized and vulcanized rubber, and improving quality control capabilities in the production process.

CN117192091BActive Publication Date: 2025-12-19ZHONGCE RUBBER GRP CO LTD +1
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Patent Information

Application Number
CN202311137656.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-05
Publication Date
2025-12-19
Estimated Expiration
2043-09-05

AI Technical Summary

Technical Problem

Traditional testing methods cannot quickly and comprehensively detect the performance of vulcanized rubber, nor can they accurately reflect the actual processing of the rubber compound, making it difficult to control product quality in a timely manner during production.

Method used

One-stop testing was performed using a rubber processing analyzer (RPA). By testing parameters such as vulcanization characteristics, hysteresis factor, and Payne effect, the vulcanization curves of unvulcanized rubber and relevant data of vulcanized rubber were obtained, including MH, ML, t50, tanδ, S*@100%, G'0.5%, G'50%, and ΔG'.

Benefits of technology

It enables rapid and comprehensive testing of rubber compound properties, and can simultaneously obtain performance data for both uncured and cured rubber, thereby improving quality control capabilities during the production process.

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Abstract

The present application relates to the technical field of rubber performance detection, and particularly relates to a performance rapid detection method, application and computer program product of silica-filled rubber. The present application can determine the vulcanization curve and vulcanization characteristics of silica-filled rubber through one-stop RPA detection, and can obtain the hysteresis factor and shear modulus of vulcanized rubber, which can help determine the dispersion of silica in rubber, and help understand the overall performance of rubber.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of rubber performance detection, and in particular to a performance rapid detection method for silica-containing rubber compound, application and computer program product. BACKGROUND

[0002] Automobile tires are extremely important in automobile components, and their performance greatly affects the handling performance and safety performance of vehicles. The performance of tires is related to the formula, and is also related to the processing process to a great extent. Therefore, the automobile design and manufacturing technology requires that more scientific and accurate quantitative data of rubber compound performance must be provided in the tire production process, so as to prove the relationship between the rubber compound characteristics and the expected processing effect and the expected product performance. Rapid detection technology can well monitor the rubber compound performance in the production process and ensure the subsequent process performance and product quality.

[0003] The actual strain, shear, temperature rise and other processes of the rubber compound in each process are actually changing all the time, and the processing process experienced by each vehicle rubber compound is different. The traditional detection involves many items such as Mooney viscosity, density, hardness, strength and curing characteristics, and uses detection instruments including rubber processing analyzer (RPA), tensile machine, dynamic mechanical analyzer, etc. The test time is relatively long, which is not conducive to the timely management and control of product quality in the factory production process. Therefore, the traditional monitoring system is a "point-to-whole" evaluation standard and evaluation result, which cannot truly reflect the true performance of the rubber compound. Therefore, a rapid rubber compound detection method is needed to realize the immediate monitoring of the production rubber compound.

[0004] In our previous patent application, two detection methods for characterizing the degree of silanization reaction were invented. Both of these two methods are based on the strain scanning data of RPA. For example, Chinese invention patent (CN109709276A, publication date: 2019-05-03) discloses that RPA is used to quantitatively calculate the degree of silanization reaction of silica in the rubber compound by the area under the G'-strain curve, which is simple to operate, has strong reproducibility and accurate judgment.

[0005] Chinese invention patent (CN107478781A, publication date: 2017-12-15) discloses a detection method for the degree of silanization reaction of silica and silane coupling agent. The method uses RPA for quantitative calculation, has strong reproducibility and accurate judgment. The mixing process of silica rubber compound can be optimized, and the same mixing process can be used to compare the degree of silanization reaction between different silica to evaluate the advantages and disadvantages between different types and different grades of silica.

[0006] However, the above method has the following disadvantages: (1) the method can only test the dispersion of white carbon black in unvulcanized rubber and the degree of silanization reaction, and cannot test the performance of vulcanized rubber; (2) the test method needs to be further optimized. SUMMARY

[0007] To solve the above technical problems, the purpose of the present application is to provide a method for rapidly detecting the performance of white carbon black-containing rubber, which can not only obtain the vulcanization curve of unvulcanized rubber through one-stop detection, but also obtain the tan δ ) and Payne effect related data of vulcanized rubber at the same time.

[0008] To achieve the above purpose, the present application adopts the following technical solutions:

[0009] A method for rapidly detecting the performance of white carbon black-containing rubber, which uses a rubber processing analyzer RPA for detection, and comprises the following steps:

[0010] 1) Test the vulcanization characteristics under the conditions of 150-190 ℃, 3-45 min, 7-42 % strain, 1-10 Hz, to obtain MH, ML and t50, and vulcanize the rubber compound at the same time;

[0011] 2) Test tan under the conditions of 55-65 ℃, 0.25-10 % strain, 5-15 Hz, and the test time is 0.1-1 min;

[0012] 3) Test at a frequency of 0.1-1 Hz under the conditions of 55-65 ℃, and the strain range is 0.28-100 %, to obtain the torque S*@100 % under 100 % strain, and the shear moduli G'0.5 % and G'50 % under 0.5 % and 50 % strain;

[0013] 4) Use the torque S*@100 % as a representation of the fixed strain, and use ΔG' to represent the Payne effect, ΔG'= G'0.5%- G'50 %.

[0014] As a preference, the white carbon black-containing rubber contains 10-150 parts by weight of white carbon black based on 100 parts by weight of pure rubber. As a further preference, the white carbon black-containing rubber contains 60-120 parts by weight of white carbon black based on 100 parts by weight of pure rubber.

[0015] As a preference, the test conditions of step 1) are 170-190 ℃, 5-15 min, 10-35 % strain, and 2-8 Hz.

[0016] As preferred, the test conditions of step 2) are 60 ℃, 3-8 % strain, 10-15 Hz, test time 0.2-0.5 min.

[0017] As preferred, the test conditions of step 2) are 60 ℃, 0.2-0.8 Hz of frequency.

[0018] Further, the application also discloses application of the performance rapid detection method of the silica white-containing rubber material in performance characterization of the silica white-containing rubber material, and torque S*100 % is used as a representation of a fixed extension stress, and ΔG' is used to represent a Payne effect.

[0019] Further, the application also discloses a computer device, including a memory, a processor and a computer program stored in the memory, and the processor executes the computer program to realize the method.

[0020] Further, the application also discloses a computer readable storage medium, which stores a computer program or instructions, and the computer program or instructions are executed by a processor to realize the method.

[0021] Further, the application also discloses a computer program product, which includes a computer program or instructions, and the computer program or instructions are executed by a processor to realize the method.

[0022] Compared with a traditional detection method, one-stop detection can obtain a vulcanization curve of a rubber material at one time, and can analyze a Payne effect and a hysteresis factor of a vulcanized rubber, has the advantages of fast testing speed, and provides an efficient means for performance control of the rubber material in a production process. Through one-stop RPA detection, a vulcanization curve and vulcanization characteristics of a silica white-filled rubber can be determined, and a hysteresis factor and a shear modulus of the vulcanized rubber can be obtained, which can help to determine dispersion of the silica white in the rubber material, and is helpful to more comprehensively understand various performances of the rubber material. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 A ΔG' curve diagram obtained through RPA detection.

[0024] Figure 2 A tanδ curve diagram obtained through RPA detection.

[0025] Figure 3 A MH / dN·m curve diagram obtained through RPA detection.

[0026] Figure 4 A S*100 % curve diagram obtained through RPA detection. DETAILED DESCRIPTION

[0027] With reference to the embodiments of the present application, the technical solutions in the embodiments of the present application will be clearly and completely described. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Under the premise of no creative labor, all other embodiments obtained by those skilled in the art based on the embodiments in the present application belong to the protection scope of the present application.

[0028] The RPA device used in the present application is RPA 2000 rubber processing analyzer produced by Alpha Technologies, USA.

[0029] The detection method comprises the following steps:

[0030] a) 180 ℃ x 5 min, 7% strain, 5 Hz, under which the vulcanization characteristics are tested to obtain MH, ML and t50, and in the process, the rubber compound is vulcanized;

[0031] b) cooling to 60 ℃, 7% strain, 12 Hz, under which tan δ is tested, and the test time is 0.3 min;

[0032] c) testing at the same temperature with a frequency of 0.5 Hz, and the strain range is 0.28-100%, under which the torque at 100% strain S*100% is tested as a representation of the modulus at a constant extension, the shear modulus at 0.5% and 50% strain (G'0.5% and G'50%) and the difference ΔG' between the two are used to represent the Payne effect.

[0033] Table 1 shows the results of the one-stop RPA detection and the traditional detection of the rubber compounds with different white carbon black formulations.

[0034]

[0035] For the vulcanization characteristic data (MH, ML and t 50 The test data of the one-stop RPA correspond to the results of the traditional MDR test, that is, the formulations with higher data in the RPA test also have higher values in the MDR test.

[0036] Since the one-stop RPA uses the torque at 100% strain S*100% to replace M100, the change rule of the two is matched, that is, the S*100% data of the one-stop RPA can be compared horizontally in different formulations.

[0037] In addition, the one-stop RPA can also obtain the Payne effect data of the vulcanized rubber, that is, Δ G ’. The above correspondence and its correlation are shown in the attached Figures 1-4 .

[0038] The foregoing is a description of the embodiments of the present application, and through the above description of the disclosed embodiments, those skilled in the art can implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art. The general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Accordingly, the present application is not to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for rapid detection of properties of silica-filled rubber compounds, which method is performed using a rubber process analyzer (RPA), characterized in that, The method comprises the following steps: 1) Cure characteristics were tested at 150 - 190 °C, 3 - 45 min, 7 - 42 % strain, 1 - 10 Hz, to obtain MH, ML and t 50 while the compound was being cured; 2) tan delta is measured at 55-65 °C, 0.25 - 10 % strain, 5 - 15 Hz, under the condition δ , test time 0.1 - 1 min; 3) 55-65 °C, test at a frequency of 0.1 -1 Hz, strain range 0.28 - 100 %, test for torque at 100 % strain S@100 %, and shear modulus at 0.5 % and 50 % strain G 0.5 % and G 50 %; 4) Torque @ 100 % is used as a representation of the set stress, Δ G Payne effect is represented by Δ G = G 0.5 % G 50 %.

2. The method for rapid detection of properties of silica white containing rubber compound according to claim 1, characterized in that, The silica-containing rubber compound has a silica addition level of 10 - 150 parts by weight based on 100 parts by weight of pure rubber.

3. The method for rapid detection of properties of silica-filled rubber compounds according to claim 1, characterized in that, The silica-containing rubber compound has a silica addition level of 60 - 120 parts by weight based on 100 parts by weight of pure rubber.

4. The method for rapid detection of properties of a silica-filled rubber compound according to any one of claims 1 to 3, characterized in that, The test conditions for step 1) are 170 - 190 °C, 5 - 15 min, 10 - 35 % strain, 2 - 8 Hz.

5. The method for rapid detection of properties of a silica-filled rubber compound according to any one of claims 1 to 3, characterized in that, The test conditions for step 2) are 60 °C, 3 - 8 % strain, 10 - 15 Hz, test time 0.2 - 0.5 min.

6. The method for rapid detection of properties of a white carbon black-containing rubber compound according to any one of claims 1 to 3, characterized in that, The test conditions for step 2) are 60 °C, 0.2 - 0.8 Hz frequency.

7. Use of a method for rapid detection of properties of a silica-filled rubber compound according to any one of claims 1 to 6 for the characterization of the properties of a silica-filled rubber compound, characterized in that, Torque at 100 % S* was used as a representation of the modulus, Δ G Payne effect was represented by the torque at 100 % S*.

8. A computer device comprising a memory, a processor, and a computer program stored on the memory, wherein the computer program comprises instructions that, when executed by the processor, cause the processor to perform the method of any one of claims 1-7. The processor executes the computer program to implement the method of any one of claims 1-6.

9. A computer readable storage medium having stored thereon a computer program or instructions, characterized in that, The computer program or instructions, when executed by the processor, implement the method of any one of claims 1-6.

10. A computer program product comprising computer programs or instructions, characterized in that, The computer program or instructions, when executed by the processor, implement the method of any one of claims 1-6.

Citation Information

Patent Citations

  • Detection method for silanizing reaction degree of white carbon blacks and silane coupling agent

    CN107478781A

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