Method for determining process conditions of white carbon black silanization reaction and application thereof

Abstract

The application discloses a method for determining process conditions of silanization reaction of white carbon black and application thereof, and relates to the technical field of rubber mixing. The method comprises the following steps: preparing a master batch containing silane coupling agent and a master batch not containing silane coupling agent by removing a vulcanization system respectively, performing temperature scanning by using a rubber processing analysis instrument, collecting a change curve of a loss factor, and judging a starting temperature of silanization reaction by comparing inflection points of two groups of curves; combining a thermal stability limit of the silane coupling agent to delimit an effective reaction temperature interval and determine a shortest constant temperature reaction duration; adding the vulcanization system again, preparing a mixed rubber by setting a plurality of groups of different gradient discharge temperatures, and vulcanizing; and testing a plurality of performances to screen and determine optimal discharge process parameters. The application also provides a method for preparing a white carbon black-containing tire mixed rubber by mixing at the discharge temperature determined by the method. The application can scientifically and accurately determine optimal process conditions of silanization reaction of white carbon black, and effectively improve the comprehensive performance of vulcanized rubber.

Description

Technical Field

[0001] This invention relates to the field of rubber compounding technology, and more specifically, to a method for determining the process conditions of silanization reaction of silica and its application. Background Technology

[0002] Silica (precipitated hydrated silica) is widely used in green tire tread compounds due to its unique reinforcing effect and ability to reduce tire rolling resistance. However, silica is rich in silanol groups (Si-OH) on its surface, exhibiting strong hydrophilicity. This results in poor compatibility with hydrophobic rubber matrices (such as natural rubber and styrene-butadiene rubber), making it difficult to disperse evenly in rubber. Consequently, the filler-rubber interfacial bonding strength is insufficient, affecting the processing performance of the compound and the physical, mechanical, and dynamic mechanical properties of the vulcanizate.

[0003] To improve the interfacial compatibility between silica and rubber, silane coupling agents are commonly used in industry for in-situ surface modification of silica, a process known as silanization. A commonly used silane coupling agent is bis-[3-(triethoxysilyl)propyl]tetrasulfide (trade name Si69), which reacts chemically with the silanol groups on the silica surface during mixing and forms chemical crosslinks with the rubber molecular chains during vulcanization, effectively improving the dispersibility and interfacial bonding strength of silica. The silanization reaction is highly sensitive to temperature and time: if the temperature is too low or the time is insufficient, the reaction is incomplete, resulting in severe silica agglomeration, increased Mooney viscosity of the rubber compound, processing difficulties, and decreased vulcanized rubber performance; if the temperature is too high or the time is too long, it can easily induce thermo-oxidative degradation of the rubber molecular chains, premature decomposition of the silane coupling agent, and the risk of scorching.

[0004] Currently, tire manufacturers rely heavily on experience to set the discharge temperature for silica compounding, lacking systematic theoretical guidance and experimental data support. This makes it difficult to guarantee the process stability and consistent performance of silica-containing rubber compounds. Therefore, there is an urgent need to establish a systematic method to scientifically determine the optimal process conditions for silanization reactions.

[0005] In view of this, the present invention is proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a method for determining the process conditions of silanization reaction of silica and its application. By scanning with a rubber processing analysis instrument system and verifying with a large-scale vehicle experiment, the starting temperature, suitable temperature range and reaction time of the silanization reaction are determined, and the optimal discharge temperature of the compound is determined accordingly, so as to improve the process stability and finished product performance of silica-containing rubber compounds.

[0007] This invention is implemented as follows: In a first aspect, the present invention provides a method for determining the process conditions for the silanization reaction of silica, comprising the following steps: Select a preset rubber base formula, remove the vulcanization system, and prepare masterbatch containing silane coupling agent and masterbatch without silane coupling agent respectively; Temperature scanning analysis was performed on the masterbatch containing silane coupling agent and the masterbatch without silane coupling agent using a rubber processing analysis instrument, and the loss factor variation curves with temperature and time were collected. The starting temperature of the silanization reaction was determined by comparing the inflection points of the loss factor change curves of the two groups of masterbatches. Based on the dynamic test data obtained from temperature scanning, combined with the thermal stability limit of silane coupling agents, the effective reaction temperature range of silanization is defined, and the shortest isothermal reaction time required to achieve the silanization reaction in this temperature range is determined. A vulcanization system was added to the rubber base formulation, and multiple batches of compounded rubber were prepared by setting multiple sets of mixing and discharge temperatures with different gradients. The compounded rubber was prepared and vulcanized separately, and multiple properties of the vulcanized rubber were tested. Based on the test data of multiple properties, the discharge temperature with the best overall performance was determined.

[0008] In an optional embodiment, the rubber base formulation comprises, by weight: 100 parts rubber matrix, 30-35 parts carbon black, and 10-20 parts silica.

[0009] In an optional embodiment, the silane coupling agent is selected as bis-[3-(triethoxysilyl)propyl]tetrasulfide, and the amount used is 2-5 parts by weight.

[0010] In an optional implementation, the temperature scan analysis is performed at a heating rate of 3-8 °C / min.

[0011] In an optional embodiment, the critical temperature for the silanization reaction is 135 °C.

[0012] In an optional embodiment, the effective reaction temperature for silanization is 135-150 °C.

[0013] In an optional embodiment, the effective silanization reaction time is 2-4 min.

[0014] In an optional embodiment, the optimal glue discharge temperature is 150 °C.

[0015] Secondly, the present invention provides a method for preparing a tire compound containing silica, wherein the compound is mixed at the discharge temperature determined by the above method, and the discharge temperature of the first stage masterbatch is ≥135 ℃.

[0016] In an optional embodiment, the compound is an all-steel radial tire tread compound.

[0017] The present invention has the following beneficial effects: (1) This invention uses a rubber processing analysis instrument to precisely scan and dynamically analyze the silanization reaction of silica, and for the first time clearly defines the starting temperature of the reaction as 135 ℃, and systematically constructs the process window of suitable reaction temperature range and optimal reaction time. This discovery completely changes the extensive mode of setting the discharge temperature based solely on operational experience in the traditional mixing process, and provides a quantitative scientific criterion for the silanization reaction process. It effectively makes up for the long-term lack of reaction kinetic parameters in this field, and shifts the control of mixing temperature from experience-dependent to data-driven, significantly improving the scientific nature and reproducibility of process setting.

[0018] (2) This invention systematically investigated the influence of different discharge temperatures on the comprehensive properties of vulcanizates, including mechanical properties, dynamic heat generation, and abrasion resistance, and determined the optimal discharge temperature under which the comprehensive properties of the vulcanizates reached the best balance. This method has a standardized operating procedure and reliable testing methods, which not only significantly improves the process stability and finished product consistency of silica-containing rubber compounds, but also has strong universality and promotional value. It can be easily transferred to the process development and optimization of other silica-rubber formulations, providing a practical and cost-effective technical path for industrial applications, with broad application prospects and significant economic and social benefits. Attached Figure Description

[0019] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 The image shows a comparison of RPA temperature scans (tanδ) for masterbatches containing and without silane coupling agents in this application. Curve 1 represents the masterbatch containing silane coupling agent, and curve 2 represents the masterbatch without silane coupling agent. Figure 2 This is a graph showing the relationship between the discharge temperature and the resilience of the vulcanized rubber in this application. Figure 3 This is a graph showing the relationship between the discharge temperature and the heat generation in the middle of the vulcanized rubber in this application. Figure 4 This is a graph showing the relationship between discharge temperature and DIN wear of vulcanized rubber in this application. Figure 5 This is a graph showing the relationship between the discharge temperature and the 100% constant tensile stress of the vulcanized rubber in this application. Figure 6 This is a graph showing the relationship between the discharge temperature and the 300% constant tensile stress of the vulcanized rubber in this application. Figure 7This is a graph showing the relationship between the discharge temperature and the tensile strength of the vulcanized rubber before aging in this application. Figure 8 This is a graph showing the relationship between the discharge temperature and the tensile strength of the vulcanized rubber after aging in this application. Figure 9 This is a graph showing the relationship between the discharge temperature and the tear strength of the vulcanized rubber before aging in this application. Figure 10 This is a graph showing the relationship between the discharge temperature and the tear strength of the vulcanized rubber after aging in this application. Figure 11 This is a graph showing the relationship between the discharge temperature and the vulcanized rubber MH in this application. Figure 12 This is a graph showing the relationship between the discharge temperature and the tanδ (70 ℃ / 10.0 Hz) of the vulcanized rubber in this application. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0022] In existing silica-filled rubber systems, the starting temperature, effective reaction temperature range, and reaction time of the silanization reaction are mostly determined through repeated trial mixing experiments based on experience. There is a lack of precise and rapid quantitative determination methods. Conventional methods of directly preparing complete vulcanizates for performance testing are superimposed with interference from the cross-linking reaction of the vulcanization system. It is impossible to isolate the interfacial reaction signal between the silane coupling agent and silica, making it difficult to accurately distinguish the performance changes caused by the silanization reaction, rubber vulcanization, and thermal degradation. The process exploration cycle is long, there are many experimental variables, and the data error is large.

[0023] Therefore, the inventors innovatively removed the vulcanization system from the basic rubber formulation in advance, and prepared two sets of masterbatches with only the single variable difference of silane coupling agent, completely eliminating the interference of vulcanization crosslinking reaction on the interfacial loss signal; by scanning with a rubber processing analyzer to obtain the loss factor (tanδ) curve, the curve of the silane-free masterbatch is flat, while the curve of the silane-containing masterbatch will show a sudden (tanδ) inflection point when the silane condensation reaction occurs. Based on this inflection point, the silanization initiation temperature is accurately determined, and then the effective reaction temperature range and reaction time are determined; then the vulcanization system is added, and the performance is measured by setting a gradient discharge temperature around the aforementioned temperature range, and the optimal discharge temperature is selected by combining the production data of the large vehicle.

[0024] Specifically, this invention discloses a method for determining the process conditions for the silanization reaction of silica, which includes the following steps: S1. Preparation of comparative masterbatch: Select a preset rubber base formula, remove the vulcanization system, and prepare masterbatch containing silane coupling agent and masterbatch without silane coupling agent respectively.

[0025] In some preferred embodiments, the rubber base formulation comprises, by weight: 100 parts rubber matrix, 30-35 parts carbon black, and 10-20 parts silica. Optionally, the basic rubber formulation may be compounded with conventional processing aids such as activators, antioxidants, and plasticizers. These processing aids do not participate in the silanization condensation reaction between the silane coupling agent and silica, and have minimal impact on the starting temperature and reaction time of the silanization reaction. This ensures that the two control masterbatches use the silane coupling agent as the only variable, and that the comparison of the tanδ curves only reflects the differences in interfacial loss caused by the silanization reaction.

[0026] Furthermore, apart from whether or not silane coupling agents are added, all other raw material components, feed amounts, and mixing processes are completely identical between the two groups of masterbatches, eliminating the interference of formulation and processing variables on the inflection point of the tanδ curve.

[0027] Preferably, the silane coupling agent is bis-[3-(triethoxysilyl)propyl]tetrasulfide (Si69), and the amount used is 2-5 parts by weight. It is understandable that various silane coupling agents will only have slight differences in the silanization initiation temperature, suitable reaction temperature range, and required reaction time corresponding to the breakpoint due to differences in molecular structure. However, this will not change the core principle of this application: "determining silanization reaction parameters by the breakpoint of the difference in tanδ curves between two control masterbatches with and without silane coupling agents". It is only necessary to repeat the RPA temperature scanning steps of this application according to the selected silane type to accurately match the optimal mixing and discharge temperature of the corresponding silane coupling agent.

[0028] S2. Rubber Processing Analyzer (RPA) Scanning Analysis: The masterbatch containing silane coupling agent and the masterbatch without silane coupling agent are subjected to temperature scanning analysis using a rubber processing analysis instrument, and the loss factor (tanδ) is collected as a function of temperature and time.

[0029] In some preferred embodiments, the temperature scanning analysis includes: heating from 100°C to 170°C at a heating rate of 3-8°C / min, and monitoring the change curve of the loss factor (tanδ) with temperature and time; the heating rate can be 3°C / min, 4°C / min, 5°C / min, 6°C / min, 7°C / min or 8°C / min, preferably 5°C / min.

[0030] It should be noted that the temperature scanning of the rubber processing analyzer is in programmed heating mode with a constant heating rate. It synchronously collects three sets of corresponding data: temperature, time, and tanδ throughout the process, and continuously plots a complete and continuous tanδ change curve.

[0031] S3. Determine the reaction initiation temperature: By comparing the inflection points of the loss factor curves of the two groups of masterbatches with temperature and time, the initiation temperature of the silanization reaction can be determined.

[0032] Specifically, as the silanization reaction proceeds, the tanδ value of the masterbatch containing the silane coupling agent gradually decreases, while the masterbatch without the silane coupling agent does not show this change. The starting temperature of the silanization reaction is determined based on the temperature at which the difference between the two occurs.

[0033] The underlying mechanism for the inflection point is as follows: below the temperature corresponding to the inflection point, there is no obvious condensation reaction between the silane coupling agent and the hydroxyl groups on the silicon surface of silica, the frictional loss at the interface between the filler and the rubber is stable, and the tanδ value fluctuates gently; after reaching the temperature corresponding to the inflection point, the alkoxy groups of the silane coupling agent and the silanol groups on the surface of silica undergo a rapid dehydration and silanization reaction, the bonding state of the filler-rubber interface changes abruptly, the frictional loss within the interface increases sharply, and the tanδ curve forms a significant upward bend at the inflection point.

[0034] In a preferred embodiment of this application, the critical temperature for the silanization reaction is 135 °C.

[0035] S4. Determine the reaction temperature range and time: Based on the dynamic test data obtained from temperature scanning, combined with the thermal stability limit of the silane coupling agent, define the effective reaction temperature range for silanization, and determine the shortest isothermal reaction time required to achieve the silanization reaction within this temperature range.

[0036] The lower limit of the suitable alkylation temperature range is the starting temperature corresponding to the tanδ inflection point; the upper limit is the critical temperature at which the difference between the tanδ values ​​of the two masterbatches no longer increases and no thermal degradation of the rubber occurs.

[0037] In some preferred embodiments, the effective reaction temperature for silanization is 135-150 °C, which can be 135 °C, 140 °C, 145 °C or 150 °C, etc.; the effective reaction time is 2-4 min, which can be 2 min, 3 min or 4 min, etc., preferably 3 min.

[0038] S5. Performance Verification: Add a vulcanization system to the rubber base formulation, set multiple sets of mixing and discharge temperatures with different gradients to prepare multiple batches of compounded rubber, prepare compounded rubber and vulcanize it respectively, and test multiple properties of the vulcanized rubber through a large vehicle test.

[0039] In some preferred embodiments, multiple properties include the physical and mechanical properties, dynamic mechanical properties, aging properties, and processing properties of the vulcanizate.

[0040] S5. Determine the optimal glue discharge temperature: Based on a comprehensive analysis of the large vehicle test data, plot the relationship curve with glue discharge temperature as the abscissa and various performance indicators as the ordinate, and determine the glue discharge temperature with the best overall performance.

[0041] In a preferred embodiment of this application, the optimal glue discharge temperature is 150 °C.

[0042] Secondly, the present invention provides a method for preparing a tire compound containing silica, comprising: adding a rubber matrix, silica, carbon black, silane coupling agent and other compounding agents into a mixing mill according to the formula ratio for mixing, and mixing at the discharge temperature determined by the above method, wherein the discharge temperature of the first masterbatch is ≥135 ℃, preferably 150 ℃.

[0043] It should be noted that silica is a difficult-to-disperse material during the mixing stage. In actual production, it is usually added together with the silane coupling agent in the first-stage masterbatch. Therefore, the silanization reaction mainly occurs in this stage, and the discharge temperature of the first-stage masterbatch needs to be carefully controlled to ensure that it falls within the suitable reaction temperature range for silane. Generally speaking, the discharge temperature of the mixing stage where the silanization reaction occurs should not be lower than 135 ℃, and it is recommended to control it at around 150 ℃ to ensure that the silane and silica fully complete the interfacial bonding. If the discharge temperature is insufficient, the silanization reaction is prone to incomplete reaction, which in turn leads to problems such as increased rolling resistance of the vulcanized rubber, poor filler dispersion, and decreased mechanical properties.

[0044] In some preferred embodiments, the compound is an all-steel radial tire tread compound.

[0045] Example 1: RPA scanning analysis to determine silanization reaction conditions In this embodiment, a basic rubber formulation was selected, and the vulcanization system was removed to prepare masterbatch containing silane coupling agent and masterbatch without silane coupling agent, respectively: The masterbatch without silane coupling agent includes: 100 parts by weight of all-steel composite rubber, 35 parts by weight of N234 carbon black, 15 parts by weight of silica, 1 part by weight of type B microcrystalline wax, 2 parts by weight of antioxidant 4020, 2 parts by weight of stearic acid, 2.5 parts by weight of F880, 0.1 parts by weight of type B plasticizer, 3.5 parts by weight of zinc oxide, and 1 part by weight of antioxidant RD.

[0046] The masterbatch containing silane coupling agent includes: 100 parts by weight of all-steel composite rubber, 35 parts by weight of N234 carbon black, 15 parts by weight of silica, 3 parts by weight of Si69, 1 part by weight of type B microcrystalline wax, 2 parts by weight of antioxidant 4020, 2 parts by weight of stearic acid, 2.5 parts by weight of F880, 0.1 parts by weight of type B plasticizer, 3.5 parts by weight of zinc oxide, and 1 part by weight of antioxidant RD.

[0047] Two masterbatches were heated from 100 °C to 170 °C at a heating rate of 5 °C / min using RPA. Temperature scanning analysis was performed, and the loss factor (tanδ) was collected as a function of temperature and time. Figure 1 As shown.

[0048] according to Figure 1 The experimental results show that the tanδ value of the silane-containing masterbatch gradually decreases as the silanization reaction proceeds, indicating that the silanization reaction consumes the silanol groups on the surface of the silica and reduces the frictional loss at the filler-rubber interface; the tanδ value of the non-silane masterbatch does not show this trend, proving that the change is indeed caused by the silanization reaction. Temperature scan curves also show that the silanization reaction begins at 135 °C and continues in the range of 135 °C-150 °C with a heating rate of 5 °C / min. The time required from the start of the reaction to its completion is approximately 3 minutes. As can be seen from the above, the starting temperature of the silanization reaction is 135 ℃, the suitable temperature range is 135 ℃-150 ℃, and the reaction time is about 3 minutes.

[0049] Example 2: Large-scale vehicle experiment to verify the properties of rubber compound at different discharge temperatures. In this embodiment, the masterbatch containing silane coupling agent from Example 1 was selected, and five groups of compound rubbers were prepared and vulcanized by setting different mixing and discharge temperatures (125℃, 140℃, 145℃, 150℃, 155℃). The various properties of the vulcanized rubbers were systematically tested, and the results are shown in Table 1.

[0050] Table 1. Test Results of Vulcanizate Performance

[0051] according to Figure 2 The results show that as the discharge temperature increases, the resilience of the vulcanized rubber gradually increases, reaching a maximum value of 58.25 at 155℃. according to Figure 3 The results show that as the discharge temperature increases, the heat generation of the vulcanized rubber gradually decreases, reaching a minimum value of 96.50 at 150 ℃. This indicates that the silanization reaction proceeds fully, the filler-rubber interface is well bonded, and energy loss under dynamic conditions is reduced. according to Figure 4The results show that the DIN abrasion value first decreases and then increases with the increase of the discharge temperature, reaching a minimum value of 127.92 at 150℃, indicating that the abrasion resistance of the rubber compound is optimal at this temperature. according to Figure 5 and Figure 6 The results show that both the 100% constant elongation stress and the 300% constant elongation stress increase with the increase of the discharge temperature, reaching the highest values ​​(3.516 MPa and 17.372 MPa) at 150℃, indicating that the silanization reaction is sufficient and the rubber-filler network structure is enhanced. according to Figure 7 and Figure 8 The results show that the tensile strength before aging increases with the increase of the discharge temperature, reaching a maximum value of 29.65 MPa at 150℃; the tensile strength after aging also shows an increasing trend. according to Figure 9 and Figure 10 The results show that the tear strength before aging gradually deteriorates with the increase of the degree of silanization reaction, reaching a minimum value of 87.57 at 150℃. This is consistent with the principle of silanization reaction—as the silanization reaction proceeds, the surface of silica changes from hydrophilic to hydrophobic, the chemical bond with rubber is strengthened, but the physical entanglement is weakened, resulting in a decrease in tear strength. After aging, the tear strength improves with the increase of the discharge temperature, and it is preliminarily speculated that the compound continues to undergo silanization reaction during the vulcanization process. according to Figure 11 The results show that MH increases with increasing debinding temperature, indicating that the silanization reaction increases the crosslinking density. according to Figure 12 The results show that after vulcanization, tanδ (70 ℃ / 10.0 Hz) decreases with increasing discharge temperature, reaching a minimum value of 0.014 at 150 ℃. This indicates that the rolling resistance of the rubber compound is the lowest at this temperature, which is most conducive to reducing tire heat generation and fuel consumption.

[0052] As can be seen from the above, the optimal temperature for discharging the compound is 150 ℃, at which point the vulcanized rubber exhibits the best overall performance.

[0053] Example 3 In this embodiment, based on the reaction process conditions determined above, the mixing and discharge temperature is set to 150 ℃ for the production of tire reinforcing rubber containing silica.

[0054] The resulting compound exhibits excellent processing stability, with minimal batch-to-batch fluctuations in Mooney viscosity, and uniform and stable dimensions in extruded and calendered semi-finished products. The finished tire filler produced by vulcanization demonstrates good dispersion, and its rolling resistance and wear resistance meet the product's preset design specifications.

[0055] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for determining the process conditions for the silanization reaction of silica, characterized in that, Includes the following steps: Select a preset rubber base formula, remove the vulcanization system, and prepare masterbatch containing silane coupling agent and masterbatch without silane coupling agent respectively; Temperature scanning analysis was performed on the masterbatch containing silane coupling agent and the masterbatch without silane coupling agent using a rubber processing analysis instrument, and the loss factor variation curves with temperature and time were collected. The starting temperature of the silanization reaction was determined by comparing the inflection points of the loss factor change curves of the two groups of masterbatches. Based on the dynamic test data obtained from temperature scanning, combined with the thermal stability limit of silane coupling agents, the effective reaction temperature range of silanization is defined, and the shortest isothermal reaction time required to achieve the silanization reaction in this temperature range is determined. A vulcanization system was added to the rubber base formulation, and multiple batches of compounded rubber were prepared by setting multiple sets of mixing and discharge temperatures with different gradients. The compounded rubber was prepared and vulcanized separately, and multiple properties of the vulcanized rubber were tested. Based on the test data of multiple properties, the discharge temperature with the best overall performance was determined.

2. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The rubber base formulation comprises, by weight, 100 parts rubber matrix, 30-35 parts carbon black, and 10-20 parts silica.

3. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The silane coupling agent is selected as bis-[3-(triethoxysilyl)propyl]tetrasulfide, and the amount used is 2-5 parts by weight.

4. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The heating rate for the temperature scan analysis is 3-8 °C / min.

5. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The critical temperature for the silanization reaction is 135 °C.

6. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The effective reaction temperature for silanization is 135-150 ℃.

7. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The effective reaction time for silanization is 2-4 min.

8. The method for determining the process conditions for the silanization reaction of silica according to claim 1, characterized in that, The optimal glue discharge temperature is 150 ℃.

9. A method for preparing a tire compound containing silica, characterized in that, The compounding is carried out using the discharge temperature determined by any one of claims 1-8, wherein the discharge temperature of the first-stage masterbatch is ≥135 ℃.

10. The method for preparing a precipitated silica-containing tire compound according to claim 9, characterized in that, The compound is a tread compound for all-steel radial tires.

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