CN109749126B - Application of bio-based renewable fatty acid ester as tread rubber plasticizer - Google Patents
Application of bio-based renewable fatty acid ester as tread rubber plasticizer Download PDFInfo
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Abstract
The invention belongs to the field of rubber auxiliary materials, and discloses an application of bio-based renewable fatty acid ester as a tread rubber plasticizer. The bio-based renewable fatty acid ester refers to fatty acid ester obtained by esterifying fatty acid with fatty alcohol or aromatic alcohol. The tread rubber comprises the following raw materials in parts by mass: 100 parts of rubber; 40-80 parts of white carbon black; 3-7 parts of a silane coupling agent; 10-20 parts of bio-based renewable fatty acid ester plasticizer; 3-5 parts of zinc oxide; 1-3 parts of stearic acid; 1-5 parts of an anti-aging agent; 0.5-2.5 parts of sulfur; 2-4 parts of an accelerator. The tread rubber using the environment-friendly bio-based renewable rubber plasticizer has low energy consumption and good plasticity in the rubber material mixing process, improves the low-temperature performance of the tread rubber on the premise of ensuring the processing performance, and keeps good physical and mechanical properties.
Description
Technical Field
The invention belongs to the field of rubber auxiliary materials, and particularly relates to an application of a bio-based renewable fatty acid ester as a tread rubber plasticizer.
Background
The rubber plasticizer is an indispensable component in the rubber manufacturing industry, particularly in the tire production, and can improve the processing performance of rubber materials and improve the physical mechanical property and the dynamic mechanical property when being applied to the tire rubber materials. The REACH regulation published in 2010 in the european union limits the use of traditional aromatic oil with high content of Polycyclic Aromatic Hydrocarbon (PAH) in tire formulations, so that it is important to find a plasticizer which can replace petroleum aromatic oil and can be applied to tire rubber materials. Under the large environment advocating the energy-saving and environment-friendly society, the environment-friendly bio-based renewable plasticizer is a necessary choice for adapting to the future technical development trend, the economic requirement and the future market development.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide the application of the bio-based renewable fatty acid ester as the tread rubber plasticizer. The bio-based renewable fatty acid ester disclosed by the invention has the advantages of no toxicity, no harm and low cost, can provide a better plasticizing effect when being applied to rubber, particularly tread rubber, endows the rubber material with excellent processability and low-temperature performance, and simultaneously keeps good physical and mechanical properties. Breaks through the defects existing in the use of the traditional plasticizer and has strong practical value.
The purpose of the invention is realized by the following technical scheme:
the application of the bio-based renewable fatty acid ester as a tread rubber plasticizer is characterized in that the bio-based renewable fatty acid ester is a fatty acid ester obtained by esterifying fatty acid with fatty alcohol or aromatic alcohol.
Preferably, the fatty acid refers to saturated fatty acid or unsaturated fatty acid with 12-24 carbon atoms.
Preferably, the fatty alcohol is monohydric alcohol or polyhydric alcohol with 1-8 carbon atoms.
Preferably, the aromatic alcohol refers to benzyl alcohol, phenethyl alcohol or benzhydrol.
Preferably, the tread rubber comprises the following raw materials in parts by mass:
preferably, the rubber is one or a mixture of more than two of natural rubber, styrene-butadiene rubber and butadiene rubber. More preferably a blend of 75 wt.% solution polymerized styrene butadiene rubber (SSBR) and 25 wt.% Butadiene Rubber (BR).
Preferably, the silane coupling agent is Si-69 (bis- [ γ - (triethoxysilyl) propyl ] tetrasulfide).
Preferably, the antioxidant is one of antioxidant RD and antioxidant 4020.
Preferably, the promoter is at least one of promoter CZ and promoter D.
Preferably, the tread rubber is prepared by the following method:
(1) first-stage mixing: at room temperature, thinly passing the rubber on an open mill for 2-8 times until the rubber is uniformly mixed;
(2) and (3) second-stage mixing: mixing the first-stage rubber compound in an internal mixer for 20-70 s at 110-130 ℃, then adding white carbon black, a silane coupling agent and a bio-based renewable fatty acid ester plasticizer for internal mixing for 60-120 s, then adding an anti-aging agent, zinc oxide and stearic acid for mixing until the temperature reaches 140-170 ℃, discharging rubber and then placing for 12-48 h;
(3) three-stage mixing: and (3) thinly passing the two-stage rubber compound on an open mill for 3-6 times at room temperature, adding sulfur and an accelerator, rolling, packaging for 3-7 times, and discharging after thinly passing to obtain the tread rubber.
Further, the speed ratio of front and rear rollers passing through the open mill in the step (1) is adjusted to be 1 (1.2-1.5); the rotating speed of a rotor of the internal mixer in the step (2) is adjusted to be 30-70 r/min; and (3) adjusting the speed ratio of the front roller and the rear roller which are thin-passed on the open mill to be 1 (1.2-1.5).
The application of the bio-based renewable fatty acid ester as the tread rubber plasticizer has the following advantages
Has the advantages that:
the application of the bio-based renewable fatty acid ester as a tread rubber plasticizer provided by the invention can provide a good plasticizing effect of rubber materials and simultaneously meet the environmental protection standard and sustainable development; the tread rubber using the environment-friendly bio-based renewable rubber plasticizer has low energy consumption and good plasticity in the rubber material mixing process, improves the low-temperature performance of the tread rubber on the premise of ensuring the processing performance, and keeps good physical and mechanical properties.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Comparative example 1
The raw material components of a general-purpose tire tread rubber material of this comparative example are shown in table 1.
TABLE 1
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer TDAE in the process, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
Example 1
The raw material components of a tire tread rubber material containing a bio-based renewable fatty acid ester plasticizer in this example are shown in table 2.
TABLE 2
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer benzyl laurate into the internal mixing chamber, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
Example 2
The raw material components of a tire tread rubber material containing a bio-based renewable fatty acid ester plasticizer in this example are shown in table 3.
TABLE 3
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer benzyl myristate in the process, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
Example 3
The raw material components of a tire tread rubber material containing a bio-based renewable fatty acid ester plasticizer in this example are shown in table 4.
TABLE 4
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer benzyl oleate in the process, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
The tire tread rubber materials prepared in the above examples 1 to 3 and comparative example 1 were subjected to a Mooney viscosity test under conditions of a large rotor, preheating at 100 ℃ for 1 minute, and heating for 4 minutes. And then carrying out mould pressing vulcanization at 160 ℃ to prepare vulcanized rubber, and then carrying out wear resistance test, mechanical property test and dynamic mechanical property test. Wherein, the mechanical property is tested according to GB/T528-2009, the dynamic mechanical property test condition is that a stretching mode is adopted, the temperature range is set to be-80-100 ℃, the temperature rise rate is 3 ℃/min, and the frequency is 10 Hz. The test results are shown in table 5.
TABLE 5
As can be seen from the results in table 5, the example formulation is compared to the comparative formulation: the mixing energy consumption is reduced, the Mooney viscosity is reduced, and the glass transition temperature of vulcanized rubber is shifted to low temperature, so that the bio-based renewable fatty acid ester plasticizer has better plasticizing effect, and the processing performance of rubber materials is improved by using the plasticizer. The elongation at break, tensile strength and 300% tensile stress of examples 1 and 2 are comparable to comparative example 1, and example 3 shows a higher elongation at break and a lower 300% tensile stress than comparative example 1. The processing performance of the tread rubber using the bio-based renewable fatty acid ester plasticizer is improved, and good physical and mechanical properties are kept.
Comparative example 2
The raw material components of a general-purpose tire tread rubber material of this comparative example are shown in table 6.
TABLE 6
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer TDEA in the process, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
Example 4
The raw material components of a tire tread rubber material containing a bio-based renewable fatty acid ester plasticizer in this example are shown in table 7.
TABLE 7
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer benzyl laurate into the internal mixing chamber, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
Example 5
The raw material components of a tire tread rubber material containing a bio-based renewable fatty acid ester plasticizer in this example are shown in table 8.
TABLE 8
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer benzyl myristate in the process, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
Example 6
The raw material components of a tire tread rubber material containing a bio-based renewable fatty acid ester plasticizer in this example are shown in table 9.
TABLE 9
The rubber material mixing adopts a three-stage mixing process, which comprises the following steps:
(1) first-stage mixing: adjusting the temperature of the open mill roller to room temperature, introducing cooling water, adjusting the speed ratio of the front roller to the rear roller to 1:1.2, and thinly passing the rubber on the open mill for 5 times;
(2) and (3) second-stage mixing: adjusting the rotating speed of a rotor of the internal mixer to be 60r/min, and the mixing temperature to be 130 ℃, putting rubber into an internal mixing chamber, and mixing for 60 seconds; then putting the white carbon black and the silane coupling agent into an internal mixing chamber, adding a plasticizer benzyl oleate in the process, and internally mixing for 90 seconds; finally, adding small materials such as an anti-aging agent, zinc oxide, stearic acid and the like into an internal mixing chamber, mixing until the temperature reaches 160 ℃, and standing for 24 hours after rubber discharge;
(3) three-stage mixing: adjusting the roll temperature of the open mill to room temperature, introducing cooling water, adjusting the speed ratio of front and rear rolls to 1:1.2, thinly passing the two-stage rubber compound on the open mill for 5 times, adding sulfur and an accelerant, rolling, packaging for 3 times, and discharging after thinly passing.
The tire tread rubber materials prepared in the above examples 4 to 6 and comparative example 2 were subjected to a Mooney viscosity test under conditions of a large rotor, preheating at 100 ℃ for 1 minute, and heating for 4 minutes. And then carrying out mould pressing vulcanization at 160 ℃ to prepare vulcanized rubber, and then carrying out wear resistance test, mechanical property test and dynamic mechanical property test. Wherein, the mechanical property is tested according to GB/T528-2009, the dynamic mechanical property test condition is that a stretching mode is adopted, the temperature range is set to be-80-100 ℃, the temperature rise rate is 3 ℃/min, and the frequency is 10 Hz. The test results are shown in table 10.
Watch 10
As can be seen from the results in table 10, the example formulation compares to the comparative formulation: the mixing energy consumption is reduced, the Mooney viscosity is reduced, and the glass transition temperature of vulcanized rubber is similar, so that the bio-based renewable fatty acid ester plasticizer has a plasticizing effect similar to or better than TDAE, the processability of rubber materials is improved by using the plasticizer, and good physical and mechanical properties can be kept.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. The application of the bio-based renewable fatty acid ester as a tread rubber plasticizer is characterized in that: the tread rubber comprises the following raw materials in parts by mass:
75 parts of solution polymerized styrene butadiene rubber;
25 parts of butadiene rubber;
55 parts of white carbon black;
the silane coupling agent is Si-694.4 parts;
3 parts of zinc oxide;
2 parts of stearic acid;
2 parts of sulfur;
1.5 parts of accelerator CZ;
1 part of an accelerator D;
40202 parts of an anti-aging agent;
20 parts of benzyl oleate.
2. The application of the bio-based renewable fatty acid ester as a tread rubber plasticizer is characterized in that: the tread rubber comprises the following raw materials in parts by mass:
100 parts of solution polymerized styrene-butadiene rubber;
55 parts of white carbon black;
the silane coupling agent is Si-694.4 parts;
3 parts of zinc oxide;
2 parts of stearic acid;
2 parts of sulfur;
1.5 parts of accelerator CZ;
1 part of an accelerator D;
40202 parts of an anti-aging agent;
20 parts of benzyl oleate.
3. The use of a bio-based renewable fatty acid ester as a tread rubber plasticizer according to claim 1 or 2, wherein said tread rubber is prepared by the following method:
(1) first-stage mixing: at room temperature, thinly passing the rubber on an open mill for 2-8 times until the rubber is uniformly mixed;
(2) and (3) second-stage mixing: mixing the first-stage rubber compound in an internal mixer for 20-70 s at 110-130 ℃, then adding white carbon black, a silane coupling agent and a bio-based renewable fatty acid ester plasticizer for internal mixing for 60-120 s, then adding an anti-aging agent, zinc oxide and stearic acid for mixing until the temperature reaches 140-170 ℃, discharging rubber and then placing for 12-48 h;
(3) three-stage mixing: and (3) thinly passing the two-stage rubber compound on an open mill for 3-6 times at room temperature, adding sulfur and an accelerator, rolling, packaging for 3-7 times, and discharging after thinly passing to obtain the tread rubber.
4. Use of a bio-based renewable fatty acid ester according to claim 1 or 2 as a tread band plasticizer, characterized in that: in the step (1), the speed ratio of the front roller to the rear roller which are thin-passed on the open mill is adjusted to 1 (1.2-1.5); the rotating speed of a rotor of the internal mixer in the step (2) is adjusted to be 30-70 r/min; and (3) adjusting the speed ratio of the front roller and the rear roller which are thin-passed on the open mill to be 1 (1.2-1.5).
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| CN113667191B (en) * | 2021-07-27 | 2023-01-10 | 中策橡胶集团股份有限公司 | Low-hardness and low-viscosity tread rubber composition, mixing method thereof and tire |
| CN114854204A (en) * | 2022-06-29 | 2022-08-05 | 广东高士高科实业有限公司 | Room-temperature vulcanized silicone rubber and preparation method and application thereof |
| CN115109170B (en) * | 2022-08-05 | 2023-11-21 | 十堰风神汽车橡塑制品有限公司 | Environment-friendly plasticizer, nitrile rubber and preparation method thereof |
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| CN101353453A (en) * | 2007-07-27 | 2009-01-28 | 铁道科学研究院金属及化学研究所 | Chloroprene rubber composition having improved cold tolerance |
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