CN112710819A - Method for evaluating flocculation reaction rate and activation energy of white carbon black in sizing material - Google Patents
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Abstract
The invention belongs to the application field of rubber industries such as tires, products and the like, and relates to a flocculation phenomenon generated in the processing processes of extrusion, vulcanization and the like of white carbon black reinforced rubber materials, and a method for calculating the reaction rate and activation energy of the phenomenon. The method comprises the steps of firstly testing time scanning of the sizing material in a rubber processing analyzer at a certain high temperature to obtain modulus change. And calculating the flocculation rate of the white carbon black at the temperature according to the modulus change. And finally, measuring the flocculation rate at more than two temperatures, and calculating the flocculation activation energy of the white carbon black according to an Arrenius equation. The evaluation method is rapid and convenient, has strong reproducibility, accurate judgment and wide application.
Description
Technical Field
The invention belongs to the application field of rubber industries such as tires, products and the like, and relates to a flocculation phenomenon generated in the processing processes of extrusion, vulcanization and the like of white carbon black reinforced rubber materials, and a method for calculating the reaction rate and activation energy of the phenomenon.
Background
In the tire industry, two main reinforcing materials of rubber are carbon black and white carbon black. Carbon black has good compatibility with olefin rubber such as natural rubber, styrene butadiene rubber and butadiene rubber due to its lipophilicity, so that the carbon black has good reinforcing effect on the rubber, and vulcanized rubber of the carbon black often has high strength and elongation at break.
White carbon black is widely used in the tire field due to its low rolling resistance and high wet grip, compared to conventional carbon black. However, white carbon black is hydrophilic and has poor compatibility with olefin rubber, and is difficult to disperse in rubber. Even if the white carbon black particles are dispersed by strong shearing in the mixing process, the dispersed white carbon black particles are flocculated together again in the subsequent processing process. And the flocculation of the white carbon black can influence the performance of the final product.
Silane coupling agent is often used to react with silicon hydroxyl on the surface of white carbon black, to improve the lipophilicity of white carbon black, improve its dispersing ability in rubber and inhibit its flocculation. However, coating the surface of the white carbon black is not complete regardless of the silane coupling agent. Therefore, the flocculation of white carbon black is unavoidable.
In the mixing process, the degree of reaction between the white carbon black and the silane coupling agent also influences the flocculation of the white carbon black. In patent CN107478781B, although a method for characterizing the degree of reaction between the two is described, the flocculation phenomenon at the later stage of the white carbon black is not studied deeply.
Disclosure of Invention
The invention provides a method for evaluating flocculation reaction rate and activation energy of white carbon black in a sizing material. The time scanning of the rubber material at a certain high temperature is tested in a rubber processing analyzer to obtain the modulus change. And calculating the flocculation rate of the white carbon black at the temperature according to the modulus change. And finally, measuring the flocculation rate at more than two temperatures, and calculating the flocculation activation energy of the white carbon black according to an Arrenius equation. The evaluation method is rapid and convenient, has strong reproducibility, accurate judgment and wide application.
The technical scheme provided by the invention for solving the technical problems is as follows:
a method for evaluating flocculation reaction rate and activation energy of white carbon black in rubber material comprises the following steps:
step 1: putting unvulcanized white carbon black reinforcing sizing material into a rubber processing analyzer, and keeping the constant temperature for 0-3 min at the temperature of 30-50 ℃;
step 2: in a rubber processing analyzer, raising the temperature to a test temperature T1, and scanning time under strain to obtain the elastic modulus G' of the rubber material at different times;
and step 3: the time scanning range is 0-60 min;
and 4, step 4: according to the time scanning result, the method is calculated according to the following formula: at a temperature T1The flocculation rate K of the white carbon black in the sizing material1：
Wherein G' (t) refers to the modulus of elasticity of the compound under strain at time t as measured using a rubber processing analyzer; g' (t)i) The elastic modulus of the rubber material under strain is measured by using a rubber processing analyzer at infinite time;
and 5: taking another sample in the same sizing material, and repeating the steps 1-4, wherein the testing temperature in the steps 2-4 is T2And calculating the flocculation rate K of the obtained white carbon black in the sizing material2；
Step 6: according to T1K of1And T2K of2And calculating the flocculation activation energy Ea of the white carbon black according to the following Arrenius equation formula:
preferably, the set strain in step 2 is 0.28 to 1.33%. More preferably, the set strain in step 2 is 0.28 to 0.56%.
Preferably, T1And T2The range of (A) should satisfy T < 60 ℃ >1＜110℃，60℃＜T2(ii) < 110 ℃; satisfy T at the same time2-T1＞10℃。
The preparation method of the unvulcanized white carbon black reinforcing rubber material comprises the following steps of:
step a: setting the rotor speed of an internal mixer to be 20-40 rpm; the initial temperature is 30-60 ℃; the filling coefficient is 0.6-0.8;
step b: adding rubber at 0 second; adding the fine materials, the silane coupling agent and the white carbon black accounting for 40-60% of the total amount in 25-35 seconds; adding the rest white carbon black when the time is 100-300 seconds; the fine materials are zinc oxide, stearic acid, an anti-aging agent and/or protective wax;
step c: adding softening oil when the temperature in the internal mixer rises to 80-110 ℃;
step d: when the temperature in the internal mixer rises to the preset silanization reaction temperature, the rotating speed of the rotor is adjusted to keep the temperature at the preset silanization reaction temperature, and the silanization reaction is carried out;
step e: and finally mixing the obtained rubber material after the reaction is finished on an open mill, adding sulfur and an accelerator, uniformly mixing and then discharging the mixture into a sheet.
Preferably, the rubber is a mixture of solution polymerized styrene-butadiene rubber and cis-butadiene rubber.
The strain of a rubber processing analyzer under 0.28-1.33% is selected, and the initial dispersion state of the filler in the rubber material is evaluated. The filler is flocculated again at high temperature in the initial dispersion state, and the flocculation intensity is influenced by the initial dispersion state and the temperature. Thus, the formula is invented
To calculate the flocculation rate at different temperatures. Finally, according to an Arrenius equation, the flocculation rates k at different temperatures T are used for calculation to obtainThe flocculation activation energy Ea of the white carbon black in the dispersion state. The smaller this flocculation activation energy value is, the more flocculation occurs.
Detailed Description
The flocculation field of the white carbon black in the processing process refers to that: during the mixing process, the white carbon black particles dispersed by the strong shearing force of the internal mixer are gathered together again under the action of high temperature mainly during the extrusion and vulcanization processes in the subsequent processing process.
The white carbon black in the invention is common white carbon black, high-dispersion white carbon black and the like produced by processes such as a precipitation method, a gas phase method and the like.
In the rubber filled with the filler such as white carbon, carbon black or the like, a network is formed between the fillers. However, the filler network gradually breaks down with increasing strain, which shows that the elastic modulus G' of the compound decreases with increasing strain, i.e. the Payne effect. Therefore, in many documents and patents, the state of dispersion of the filler is characterized using a rubber compound at a low strain modulus.
Literature (Investigation and Improvement of the Scorp beer of silicon-filled solvent Rubber Compound. journal of Applied Polymer science.2019,136(35): 47918-.
Example 1
Evaluating and calculating different formulas and different mixing processes to prepare the white carbon black reinforcing sizing material white carbon black flocculation activation energy.
Schemes 1-6, the formulation and mixing process of comparative example 1 are described in table 1:
TABLE 1
| Formulation (phr parts) | Scheme 1 | Scheme 2 | Scheme 3 | Scheme 4 | Scheme 5 | Comparative example 1 | Comparative example 2 |
| Solution polymerized styrene-butadiene rubber | 75 | 75 | 75 | 75 | 75 | 75 | 75 |
| Cis-butadiene rubber | 25 | 25 | 25 | 25 | 25 | 25 | 25 |
| White carbon black 1165MP | 80 | 80 | 80 | 80 | 80 | 0 | 0 |
| Carbon black | 0 | 0 | 0 | 0 | 0 | 80 | 80 |
| Silane coupling agent Si69 | 6.4 | 6.4 | 6.4 | 6.4 | 6.4 | 6.4 | 0 |
| Silane coupling agent Si75 | 0 | 0 | 0 | 0 | 0 | 0 | 6.4 |
| Softening oil | 32.5 | 32.5 | 32.5 | 32.5 | 32.5 | 32.5 | 32.5 |
| Others | 10.7 | 10.7 | 10.7 | 10.7 | 10.7 | 10.7 | 10.7 |
| Total parts of | 229.6 | 229.6 | 229.6 | 229.6 | 229.6 | 229.6 | 229.6 |
| Silanization holding temperature/. degree.C | 150 | 150 | 150 | 140 | 140 | 150 | 150 |
| Silanization retention time/s | 60 | 120 | 180 | 120 | 180 | 120 | 120 |
The raw materials used in the formula are detailed:
solution polymerized styrene butadiene rubber, 4526-2HM, langsheng chemical product;
cis-butadiene rubber, BR9000, a product of the daqing petrochemical division of medium petroleum;
white carbon black, 1165MP, solvay chemical products;
carbon black, N234, cabot product;
silane coupling agent, Si69, conifer chemical;
silane coupling agent, Si75, conifer chemical;
softening oil, TDAE, hansheng chemical products; the rest raw materials are commercial industrial products.
The 7 formulas are respectively put into an internal mixer for mixing, the schemes 1 to 5 and the comparative examples 1 to 2 use the same process for mixing,
the method comprises the following specific steps:
(a) setting the rotating speed of a rotor of the internal mixer to be 40 rpm; the initial temperature is 60 ℃; the filling factor is 0.7;
(b) all rubber was added at 0 second; adding 1/2 total amount of white carbon black, zinc oxide, stearic acid, anti-aging agent,
Protective wax, and adding the rest white carbon black when 60 seconds;
(c) adding softening oil when the temperature of the internal mixer rises to 95 ℃;
(d) when the temperature of the internal mixer rises to the temperature of the silylation reaction corresponding to the scheme, the rotating speed of the rotor is adjusted to keep the temperature at the temperature of the silylation reaction corresponding to the scheme for the silylation reaction, and the reaction time is the silylation reaction time preset in the scheme 1-5 respectively;
the method comprises the following steps that 1, silane Si69 is used, the silanization reaction temperature is 150 ℃, and the preset reaction time is 60 s; .
The scheme 2 adopts silane Si69, the silanization reaction temperature is 150 ℃, and the preset reaction time is 120 s;
silane Si69 is used in the scheme 3, the silanization reaction temperature is 150 ℃, and the preset reaction time is 180 s;
scheme 4 uses silane Si69, the silylation reaction temperature is 140 ℃, and the preset reaction time is 120 s;
scheme 5 uses silane Si69, the silylation reaction temperature is 140 ℃, and the preset reaction time is 180 s;
in comparative examples 1 to 2, carbon black was used instead of silica, although the silylation reaction between silica and silane did not occur. But by contrast, still at a temperature of 150 ℃, for 120 s;
(e) after the reaction is finished, rubber is discharged, the rubber material is finally refined on an open mill, sulfur (10 percent of oil-filled sulfur powder, a tin-free lush product) and an accelerator (an accelerator CZ, a Shandong Shunhui product) are added, the mixture is uniformly mixed and then is discharged, and the mixture is kept stand for 8 hours.
Testing the rubber processing analyzer:
step 1: the test is carried out in a rubber processing analyzer, and the unvulcanized white carbon black reinforced rubber material is put into the rubber processing analyzer and is kept for 1min at the constant temperature of 40 ℃.
Step 2: in a rubber processing analyzer, the temperature is raised to 80 ℃, time scanning is carried out under the strain of 0.28 percent, the scanning time is 30min, and the elastic modulus G' of the rubber material under different strains is obtained.
And 4, step 4: according to the time scanning result, the flocculation rate K1 of white carbon black in the sizing material at 80 ℃ (353K) is calculated according to the following formula:
g 'in the formula'0.28(t) refers to the modulus of elasticity of the compound at 0.28% strain at time t, measured using RPA 2000. G'0.28(t30) Refers to the modulus of elasticity of the compound at 0.28% strain measured at infinity using RPA 2000.
And 5: taking another sample in the same rubber material, and repeating the steps 1-4 to obtain the temperature T2The flocculation rate K of the white carbon black in the sizing material2。
The flocculation rate K and the flocculation activation energy Ea at 80 ℃ and 100 ℃ for schemes 1 to 5 and comparative examples 1 and 2 (absolute temperatures 353K and 373K, respectively) are shown in Table 2.
TABLE 2
Example 2
Example 2 the flocculation activation energy of white carbon black of the same formulation and different specific surface areas was evaluated and calculated.
Generally, the smaller the particle size of white carbon, the larger the surface energy thereof, and the faster the coagulation rate. Example 2 the flocculation activation energy of different specific surface areas of silica was evaluated.
Wherein, the surface area of the white carbon black is measured by using a CTAB method, and the selected white carbon black and the corresponding specific surface area are as follows: 1165MP, CTAB value 170; 1115MP with a CTAB value of 120; 200MP and CTAB is 200. The three white carbon blacks are all products of Sorvey company.
The formulation and silylation reaction conditions used in example 2 are shown in table 3. The rest of the mixing process was the same as in example 1.
TABLE 3
| Formulation (phr parts) | Scheme 1 | Scheme 6 | Scheme 7 |
| Solution polymerized styrene-butadiene rubber | 75 | 75 | 75 |
| Cis-butadiene rubber | 25 | 25 | 25 |
| White carbon black 1165MP | 80 | 0 | 0 |
| White carbon black 1115MP | 0 | 80 | 0 |
| White carbon black 200MP | 0 | 0 | 80 |
| Silane coupling agent Si69 | 6.4 | 6.4 | 6.4 |
| Softening oil | 32.5 | 32.5 | 32.5 |
| Others | 10.7 | 10.7 | 10.7 |
| Total parts of | 229.6 | 229.6 | 229.6 |
| Silanization holding temperature/. degree.C | 150 | 150 | 150 |
| Silanization retention time/s | 60 | 60 | 60 |
The flocculation rate K values at 80 ℃ and 100 ℃ (corresponding to absolute temperatures of 353K and 373K, respectively) for schemes 1-5 and comparative examples 1 and 2 are shown in Table 4.
TABLE 4
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention, including any reference to the above-mentioned embodiments. Various modifications to these embodiments will be readily apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended 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 (6)
1. The method for evaluating the flocculation reaction rate and the activation energy of white carbon black in rubber is characterized by comprising the following steps of:
step 1: putting unvulcanized white carbon black reinforcing sizing material into a rubber processing analyzer, and keeping the constant temperature for 0-3 min at the temperature of 30-50 ℃;
step 2: in the rubber processing analyzer, the temperature is raised to a test temperature T1Scanning time under strain to obtain the elastic modulus G' of the rubber material at different times;
and step 3: the time scanning range is 0-60 min;
and 4, step 4: according to the time scanning result, the method is calculated according to the following formula: at a temperature T1The flocculation rate K of the white carbon black in the sizing material1：
Wherein G' (t) refers to the modulus of elasticity of the compound under strain at time t as measured using a rubber processing analyzer; g' (t)i) The elastic modulus of the rubber material under strain is measured by using a rubber processing analyzer at infinite time;
and 5: taking another sample in the same sizing material, and repeating the steps 1-4, wherein the testing temperature in the steps 2-4 is T2And calculating the flocculation rate K of the obtained white carbon black in the sizing material2；
Step 6: according to T1K of1And T2K of2And calculating the flocculation activation energy Ea of the white carbon black according to the following Arrenius equation formula:
2. the method for evaluating the flocculation reaction rate and the activation energy of white carbon black in a rubber compound according to claim 1, wherein the set strain in the step 2 is 0.28-1.33%.
3. The method for evaluating the flocculation reaction rate and the activation energy of white carbon black in a rubber compound according to claim 1, wherein the set strain in the step 2 is 0.28-0.56%.
4. The method for evaluating the flocculation reaction rate and activation energy of white carbon black in rubber compound according to claim 1, wherein T is T1And T2The range of (A) should satisfy T < 60 ℃ >1＜110℃，60℃＜T2(ii) < 110 ℃; satisfy T at the same time2-T1＞10℃。
5. The method for evaluating the flocculation reaction rate and activation energy of white carbon black in a compound according to claim 1, wherein the method for preparing the unvulcanized white carbon black reinforced compound comprises the following steps:
step a: setting the rotor speed of an internal mixer to be 20-40 rpm; the initial temperature is 30-60 ℃; the filling coefficient is 0.6-0.8;
step b: adding rubber at 0 second; adding the fine materials, the silane coupling agent and the white carbon black accounting for 40-60% of the total amount in 25-35 seconds;
adding the rest white carbon black when the time is 100-300 seconds; the fine materials are zinc oxide, stearic acid, an anti-aging agent and/or protective wax;
step c: adding softening oil when the temperature in the internal mixer rises to 80-110 ℃;
step d: when the temperature in the internal mixer rises to the preset silanization reaction temperature, the rotating speed of the rotor is adjusted to keep the temperature at the preset silanization reaction temperature, and the silanization reaction is carried out;
step e: and finally mixing the obtained rubber material after the reaction is finished on an open mill, adding sulfur and an accelerator, uniformly mixing and then discharging the mixture into a sheet.
6. The method for evaluating the flocculation reaction rate and activation energy of white carbon black in a rubber material according to claim 1, wherein the rubber is a mixture of solution polymerized styrene-butadiene rubber and cis-butadiene rubber.
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| CN113607934A (en) * | 2021-06-18 | 2021-11-05 | 中策橡胶集团有限公司 | Evaluation method and equipment for white carbon black sizing material vulcanization process and computer readable carrier medium |
| CN113960297A (en) * | 2021-09-17 | 2022-01-21 | 中策橡胶集团有限公司 | Method, equipment and computer program product for evaluating flocculation rate of white carbon black reinforced sizing material |
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| CN113607934A (en) * | 2021-06-18 | 2021-11-05 | 中策橡胶集团有限公司 | Evaluation method and equipment for white carbon black sizing material vulcanization process and computer readable carrier medium |
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| CN113960297A (en) * | 2021-09-17 | 2022-01-21 | 中策橡胶集团有限公司 | Method, equipment and computer program product for evaluating flocculation rate of white carbon black reinforced sizing material |
| CN113960297B (en) * | 2021-09-17 | 2023-09-26 | 中策橡胶集团股份有限公司 | Method, equipment and computer program product for evaluating flocculation rate of white carbon black reinforced sizing material |
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