Fig 1 Schematic illustration of loading antioxidant 4010NA into SAG.
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网络出版日期:2024-04-25,
收稿日期:2023-12-04,
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录用日期:2024-03-11
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The antioxidant N-isopropyl-N'-phenyl-p-phenylenediamine (4010NA) was dissolved in ethanol and impregnated into silica aerogel (SAG) via vacuum-pressure cycles, yielding composite particles (A-N) with enhanced sustained-release and reinforcing capabilities. The effect of A-N on the mechanical properties and thermal-oxidative aging resistance of styrene-butadiene rubber (SBR) vulcanizates was investigated. TGA and BET assessments indicated that the loading efficiency of 4010NA in SAG reached 14.26% within ethanol's solubility limit. Incorporating A-N into SBR vulcanizates significantly elevated tensile strength by 17.5% and elongation at break by 41.9% over those with fumed silica and free 4010NA. Furthermore, A-N notably enhanced the thermal-oxidative aging resistance of SBR. After aging for 96 h at 100 °C, the tensile strength and elongation at break of SBR with A-N sustained 70.09% and 58.61% of their initial values, respectively, with the retention rate of elongation at break being 62.8% higher than that of SBR with fumed silica and free antioxidant. The study revealed that A-N composite particles significantly inhibited the crosslinking in SBR's molecular chains, reducing hardening and embrittlement during later thermal-oxidative aging stages.
In this study, composite particles (A-N) with both slow-release and reinforcing functions were obtained by loading the antioxidant into the pores of silica aerogel powders. Thermo-oxidative aging of vulcanized rubber was inhibited by continuous release of antioxidant from A-N.
Rubber, due to its outstanding elasticity and insulating characteristics, is acknowledged as a strategic material globally.[
The most prevalent method of preventing thermal-oxidative aging in rubber involves the addition of chemical antioxidants. These antioxidants react with active substances like oxygen and ozone, effectively inhibiting rubber aging. That's why maintaining a continuous supply of antioxidants throughout the service period of rubber materials is crucial in extending their service life.[
Chemical grafting of antioxidant to the surface of filler,[
Silica aerogel (SAG), a porous material, boasts a three-dimensional network structure constituted by nano-sized silica particles. The material is renowned for its extraordinary porosity and minimal thermal conductivity.[
In this study, N-isopropyl-N'-phenyl-p-phenylenediamine (4010NA), an antioxidant, was dissolved in ethanol and incorporated into the pores of SAG via multiple cycles of negative and normal pressure. This resulted in composite particles (A-N) with sustained-release antioxidant and reinforcing capabilities. The effects of these composite particles on the thermal-oxidative aging resistance of SBR vulcanizates were thoroughly examined. This was achieved by comparing the changes in mechanical properties, characteristic functional group content, and crosslinking density of SBR vulcanizates before and after thermal-oxidative aging. The mechanism of thermal-oxidative aging resistance was also analyzed.
The following materials were procured for this study. Styrene-butadiene rubber (SBR1712) from Sinopec Qilu Company, zinc oxide (CR) from Liuzhou Zinc Company, stearic acid from Fengyi Oil and Fat Technology Company, and antioxidant 4010NA (effective component content, 98%) from Shandong Shangshun Chemical Company. Additionally, silica aerogel, with trademark AG-D, was sourced from Huayang New Material Technology Group Co. Ltd., while fumed silica was procured from Cabot (Tianjin). Absolute alcohol (AR) was sourced from Tianjin Tianli Chemical Reagent Co., Ltd.
The process for preparing silica aerogel-loaded antioxidant 4010NA composite particles, denoted as “A-N” in this study, is illustrated in
Fig 1 Schematic illustration of loading antioxidant 4010NA into SAG.
According to the formula in
Sample | SBR (phr) | A-N (phr) | SAG (phr) | 4010NA (phr) | Fumed silica (phr) |
---|---|---|---|---|---|
S45 | 100 | 0 | 0 | 0 | 45 |
S30A15 | 100 | 0 | 15 | 0 | 30 |
S45N1 | 100 | 0 | 0 | 1 | 45 |
S30A15N1 | 100 | 0 | 15 | 1 | 30 |
S30A8A-N8 | 100 | 8 | 8 | 0 | 30 |
S30A8N0.5A-N8 | 100 | 8 | 8 | 0.5 | 30 |
Cross-link density measurement
The crosslinking density (Ve) of vulcanizates was tested by swelling method.[
1
where Ve is the cross-link density of the rubber (measured in mol/cm³). V0 is the molar volume of the solvent (expressed in ml/mol). X is the interaction parameter between the rubber and solvent, which is estimated by Eq. (2):
2
where Vr is the volume fraction of rubber in the swollen sample, determined by Eq. (3):
3
The parameters in the formula are defined as follows: ρs represents the density of the solvent, denoted in grams per cubic centimeter (g/cm³). Wd refers to the weight of the unaltered rubber specimen, recorded in grams (g). Meanwhile, Ws signifies the weight of the rubber sample post-immersion in the solvent and subsequent drying to eliminate any surface solvent, also quantified in grams (g).
Morphological analysis
The surface morphology of the samples was examined using a scanning electron microscope (GEMINISEM 360, ZEISS, Germany).
Chemical structural analysis
The absorption peaks of the characteristic functional groups of all the samples were characterized by a Fourier-transform infrared spectrometer (INVENIO-S, Bruker Corporation, Germany).
Measurement of loading efficiency of 4010NA on silica aerogel
Thermogravimetric analyzer (TGA2, METTLER TOLEDO, Switzerland) was used to test the thermal weight loss of composite particles in the temperature range of 30−900 °C by a heating rate of 10 °C / min in a nitrogen atmosphere. The loading efficiency (Ca) of 4010NA in SAG was calculated according to Eq. (4),[
4
where wA-N is weight loss rate (%) of composite particles at 900 °C, wSAG is weight loss rate (%) of raw silica aerogels.
Specific surface area and pore size analysis
The nitrogen adsorption and desorption curves of raw SAG and composite particles were tested at 100 °C by an automatic surface area and porosity analyzer (Quantachrome Autosorb IQ, Quantachrome Instruments U.S, USA). The pore size distribution and specific surface area were analyzed.
Vulcanization characteristics testing of rubber materials
The vulcanization characteristics of rubber compounds were tested by a rotorless vulcanizer (MDR 3000 Basic, MonTech, Germany). The test temperature was 160 °C and the duration time was 60 min.
Mechanical properties testing of rubber vulcanizates before and after aging
Samples after thermal oxidative aging were obtained under the following conditions: In accordance with ISO 188:2011, dumbbell-shaped specimens were placed in a thermal-oxidative aging oven (401B, Yangzhou Tianfa Testing Machinery Co., Ltd., China) at 100 °C within an air atmosphere for various durations.
The tensile properties of the vulcanizate samples before and after aging were tested at room temperature according to ISO 37:2017 using a universal testing machine (UTM4304X, Shenzhen Sansi Zongheng Technology Co. Ltd., China). The tensile speed was set to 500 mm/min.
Glass transition temperature testing of rubber vulcanizates
The glass transition temperature of the rubber vulcanizates, both before and after aging, was characterized using a dynamic thermomechanical analyzer (DMA 242 E Artemis, NETZSCH, Germany).
Surface hydrophobicity testing of rubber materials
The surface hydrophilicity of rubber vulcanizates was characterized using an optical contact angle measuring instrument (DSA100S, KRUSS, Germany).
Other components: Zinc oxide, 5 phr (parts per hundred rubber); Stearic acid, 1 phr; CZ accelerator, 1 phr; DM accelerator, 1 phr; Sulfur, 4 phr.
Scanning electron microscopy (SEM) was employed to examine the morphology of the SAG and A-N composite particles, as demonstrated in Fig. S1 (in the electronic supplementary information, ESI). It can be observed that the size of the SAG particles used is approximately 3−5 μm. After the loading with 4010NA, the three-dimensional structural morphology of the SAGs remained intact.
To further delve into the possibility of any chemical reactions taking place during the loading of antioxidant 4010NA into the SAG pores, Fourier-transform infrared spectroscopy (FTIR) was performed on both SAG and A-N composite particles. The results of these examinations are exhibited in Fig. S2 (in ESI). As shown in Fig. S2 (in ESI), FTIR curves show the signal of residual small alkanes from the preparation of SAG.[
The antioxidant-silica aerogel (A-N) composite particles utilized in this research were prepared through the process of impregnating SAG with a 4010NA ethanol solution, followed by vacuum treatment. To ascertain the impact of 4010NA concentration within the ethanol solution on the overall loading efficiency, a thermogravimetric analyzer was employed to chart the thermal weight loss curve of the composite particles within a nitrogen environment. The resultant data is illustrated in
Fig 1 TGA curves of SAG and A-N composite particles prepared using different concentrations of (a) 4010NA ethanol solution and (b) 4010NA loading efficiency.
The loading efficiency (Ca) of 4010NA within SAG was determined through the experimental method outlined earlier, as illustrated in
The pore volume and specific surface area of SAG, before and after 4010NA loading, were evaluated using an automated surface area and pore size analyzer. The nitrogen adsorption-desorption isotherms and pore size distribution curves for SAG and A-N composite particles, with varying 4010NA content, are presented in Fig. S3 (in ESI). An analysis of the pore structure data for the different A-N composite particles are shown in
Sample | Pore volume (cm3·g−1) | Specific surface area (cm2) | Pore diameter (nm) |
---|---|---|---|
SAG | 0.994 | 492.73 | 30.37 |
3% | 1.136 | 472.94 | 35.75 |
6% | 1.132 | 444.70 | 35.60 |
9% | 1.092 | 439.89 | 35.82 |
12% | 1.146 | 439.62 | 35.67 |
As specified in
The torque curves as a function of time during the vulcanization process for these six compounds were tested at 160 °C, as demonstrated in
Fig 2 Time-dependent dynamic torque curves at 160 °C for diverse SBR compounds.
Sample | MH (dN·m) | ML (dN·m) | tc10 (min) | tc90 (min) | ΔM (dN·m) |
---|---|---|---|---|---|
S45 | 20.10 | 2.21 | 4.84 | 12.26 | 17.89 |
S30A15 | 19.92 | 2.45 | 5.49 | 11.99 | 17.47 |
S45N1 | 18.09 | 1.79 | 4.24 | 9.75 | 16.30 |
S30A15N1 | 18.47 | 2.12 | 4.71 | 10.87 | 16.35 |
S30A8A-N8 | 19.37 | 2.28 | 2.27 | 6.59 | 17.09 |
S30A8N0.5A-N8 | 16.07 | 2.40 | 2.25 | 6.62 | 13.67 |
Note: MH, maximum torque;ML, minimum torque; tc10, time at 10% vulcanization; tc90, time at 90% vulcanization; ΔM = MH − ML.
The incorporation of A-N composite particles notably decreases tc10 without a significant reduction in ΔM. The subsequent introduction of free 4010NA to S30A8A-N8 results in a further diminution of both tc10 and ΔM. This is attributed to the fact that when antioxidant 4010NA is integrated into the pores of SAG, it is predominantly bound by SAG, resulting in a more evenly distributed dispersion within the system and consequently leading to a further decrease in tc10. The confinement of 4010NA within the pores substantially minimizes its decomposition during processing, consequently mitigating its detrimental effects on cross-linking. Further addition of free 4010NA to S30A8A-N8 can reduce its tc10 and ΔM even more.
The extensive incorporation of antioxidants in conventional rubber formulations leads their migration to the surface of vulcanizates, resulting in the phenomenon of frosting that markedly impairs the mechanical properties. These antioxidants are typically low-molecular-weight, hydrophobic compounds whose accumulation at the vulcanized rubber's surface augments its hydrophobicity—a factor that inversely correlates with anti-frosting efficacy.[
Fig 3 SEM micrographs detailing the surface morphology of SBR/A-N vulcanizates placed for 60 days at ambient temperature.
The SEM images demonstrate that the surfaces of S45 and S30A15, devoid of unbound 4010NA, are notably smooth, suggesting an absence of antioxidant migration. In contrast, the surfaces of S45N1 and S30A15N1 exhibit layered aggregates, indicative of migrated antioxidants. However, S30A8A-N8 and S30A8N0.5A-N8 retain their smoothness, implying negligible antioxidant migration.
The hierarchy of water contact angles among the six groups of samples, in descending order, is S45N1, S30A15N1, S30A8N0.5A-N8, S30A15, S30A8A-N8, and S45. The SAG employed in these formulations contains residual organic constituents, contributing to a degree of hydrophobicity that results in a greater water contact angle for S30A15 compared to S45. The hydrophobic organic compound 4010NA, when migrated to the vulcanizate's surface, further enhances hydrophobicity, as evidenced by the highest contact angle observed in S45N1. The marginally lower angle in S30A15N1 is attributed to partial adsorption of free 4010NA by the SAG. The surface of S30A8A-N8 is largely free of migrated antioxidants owing to the robust binding affinity of SAG, which is reflected in a water contact angle only slightly elevated compared to the antioxidant-free S45. For S30A8N0.5A-N8, the presence of additional unbound antioxidant increases the contact angle beyond that of S30A8A-N8, as the saturated A-N composite particles are incapable of adsorbing the excess antioxidants.
The six SBR compounds previously described were subjected to thermal vulcanization at 160 °C, utilizing a tc90+5 min protocol, to yield a series of vulcanized SBR materials. These vulcanizates were fashioned into dumbbell-shaped specimens and subjected to thermal-oxidative aging at 100 °C for varying durations (24 h, 72 h, 96 h) within a controlled aging chamber.
The original stress-strain curves for six sets of samples before and after aging for various durations are shown in
Fig 4 The original stress-strain curves of SBR/A-N vulcanizates before and after thermal-oxidative aging at 100 °C for various period (a: 0 h; b: 24 h; c: 72 h; d: 96 h).
Fig 5 The tensile modulus (a) and stress at 100% (b) of SBR/A-N vulcanizates before and after thermal-oxidative aging at 100 °C for various timeframes.
Fig 6 (a−c) Mechanical properties, (d, e) retention rates, and (f) the rate of increase in hardness of SBR/A-N vulcanizates before and after thermal-oxidative aging at 100 °C for various timeframes.
From
After undergoing aging at 100 °C for 24 h, the sample S30A15 demonstrates a more significant enhancement in tensile modulus relative to sample S45. Conversely, the rise in tensile stress at 100% elongation for S30A15 is less marked. Consequently, S30A15 surpasses S45 in maintaining tensile strength and elongation at break by margins of 22.65% and 11.64%, respectively. This is attributed to the high structural integrity of SAG, making the interaction between SAG and SBR more robust and less prone to disruption. The addition of SAG enhances the early-stage thermal-oxidative aging resistance of SBR, which is not observed in carbon nanotube (CNT)-reinforced SBR.[
After aging at 100 °C for 96 h, the S30A8A-N8 sample containing A-N retained 43.88% of its initial elongation at break, which is higher than the 33% for the control group S45 and S30A15, and 36% for S45N1 and S30A15N1. This is attributed to the continuous and sustained release of antioxidants from the mesopores of SAG as aging time increases. In the case of the sample S30A8N0.5A-N8, which contains both free antioxidants and A-N, free antioxidants are consumed in the early stages of aging. In the subsequent aging process, encapsulated 4010NA within the A-N composite continues to be released, mitigating further cross-linking of the rubber molecular chains and efficiently maintaining the elongation at break of the sample (elongation at break retention of 58.61% after 96 h of aging), reducing the increase in hardness. Consequently, this minimizes the decrease in tensile strength to the maximum extent.
The thermal-oxidative degradation of rubber typically proceeds as follows (refer to
Fig 2 The mechanism of A-N releasing antioxidant and improving the thermal oxidative aging resistance of SBR vulcanizate.
To investigate the thermal-oxidative aging resistance of SBR/A-N vulcanizates, we performed infrared spectroscopy testing on six sets of samples subjected to aging over varied durations. The infrared spectra of these sample at different aging intervals are presented in Fig. S5 (in ESI). For a clearer representation of the thermal-oxidative aging resistance, we computed the carbonyl index (CI) as shown in
Fig 7 Changes in characteristic functional group parameters of SBR/A-N vulcanizates with aging time. (a) Variation of CI values with aging time at 100 °C; (b) Variation of CI values with aging time at 150 °C; (c) Variation of methylene retention rate at 1447 cm−1 with aging time at 150 °C.
5
The trend of methylene retention rates during aging at 150 °C, depicted in
During thermal-oxidative aging, the extensive generation of free radicals from molecular chain scission prompts increased cross-linking. This augmentation of cross-link density curtails the mobility of polymer chain segments, diminishing their flexibility, which can be evidenced by an elevation in the glass transition temperature (Tg).[
Fig 8 (a) tanδ-temperature curves for the unaged samples and (b) the Tg evolution rate with aging time for the six sets of samples.
As indicated in
Moreover, the impact of thermal-oxidative aging on the Tg of different samples was assessed. The tanδ transitions with temperature for the six aged samples are presented in Fig. S6 (in ESI), and the corresponding Tg growth rates with aging time are depicted in
During the thermal-oxidative aging of SBR, concurrent chain scission and cross-linking significantly modify the polymer's molecular structure. It has been observed that re-crosslinking during aging primarily contributes to the rise in the Tg and the associated changes in mechanical properties.[
To intuitively assess changes in the crosslinking density (Ve) of samples before and after thermal-oxidative aging, Ve was tested through equilibrium swelling methods and the results were normalized and presented in
Fig 9 Variation of crosslink density (Ve) with aging time for six groups of samples.
In the initial stage of aging, all six sets of samples exhibited a rapid increase in Ve corresponding with the duration of aging. Nonetheless, the Ve increase for S45N1 and S30A15N1 was less pronounced than that for S45 and S30A15 throughout the aging process. In contrast, samples containing A-N composites (S30A8A-N8) and those with both free antioxidants and A-N composites (S30A8N0.5A-N8) showed a reduction in Ve after aging 100 h. This trend is in line with the aforementioned Tg observations, reinforcing the premise that crosslinking predominates as the key reaction mechanism for SBR molecular chains during the later stages of thermal-oxidative aging.
During the aging process of rubber, antioxidants play a crucial role in mitigating the increase of Ve by scavenging free radicals. As a result, samples S45 and S30A15, which lack antioxidants, exhibit a rise in Ve that correlates with the duration of aging. Conversely, samples S45N1 and S30A15N1, containing free antioxidants, show a reduced rate of Ve increase, attributable to the antioxidants' radical-capturing activity. The samples S30A8A-N8 and S30A8N0.5A-N8, with a lower content of free antioxidants compared to S30A15N1, exhibit a less pronounced inhibition of the cross-linking reaction in the initial stages of aging. Consequently, the early aging stage sees a more significant increase in Ve for these samples than for S30A15N1. However, as the aging progresses, the sustained release of antioxidants from the A-N composites maintains the inhibition of cross-linking. In the latter stages, the degradation of macromolecules becomes more pronounced, leading to a progressive reduction in the Ve of S30A8A-N8 and S30A8N0.5A-N8.
In summary, the thermal-oxidative aging resistance mechanism of SBR reinforced by A-N composite particle can be illustrated as in
In this study, silica aerogels (SAG) were utilized as carriers to develop composite particles that serve dual functions: sustained release of antioxidants and reinforcement of the polymer matrix. Incorporating these composite particles into the styrene-butadiene rubber (SBR) matrix enhanced the antioxidant concentration by 150% without any observable migration. This augmentation resulted in significant enhancements in the mechanical properties of the SBR vulcanizates evidenced by the fact that, the tensile strength and elongation at break of vulcanizates containing A-N composite particles (S30A8N0.5A-N8) were increased by 17.5% and 41.9%, respectively, in contrast to those with fumed silica and unencapsulated antioxidants (S45N1).
Most notably, the addition of 4010NA-loaded SAG markedly improved the thermal-oxidative aging resistance of the SBR vulcanizates. After 96 hours of aging, the tensile strength and elongation at break of S30A8N0.5A-N8 samples retained 70.09% and 58.61% of their original values, respectively. Compared to the S45N1 samples, the retention rate of elongation at break was 62.8% higher, signifying that the A-N composite particles effectively curtailed the intermolecular cross-linking reactions that typically occur in the later stages of thermal-oxidative aging.
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