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Preparation of natural raw rubber and silica/NR composites with low generation heat through aqueous silane flocculation

  • Pengfei Diao , Yao Xiao , Zheng Gong , Shenglong Yang , He Wang , Chuansheng Wang EMAIL logo and Huiguang Bian
Published/Copyright: December 31, 2024
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e-Polymers
From the journal e-Polymers Volume 24 Issue 1

Abstract

An aqueous aminosilane oligomer, Crosile® 8150 (hereinafter referred to as 8150) was introduced to flocculate natural rubber latex, realizing the preparation of natural raw rubber and natural rubber composites. Compared with smoked rubber, the natural raw rubber flocculated with 2, 4, and 6 phr 8150 exhibited lower glass transition temperatures, enhancing the flexibility of the molecular chain, improving the plasticity retention rates by 18.32%, 1.75%, and 22.18%, respectively, and increasing the resistance to thermo-oxidative aging. The silica/natural rubber composites prepared from natural dry rubber prepared by 8150 flocculation had superior rolling resistance properties compared to smoked rubber. The application of 8150 in the preparation of natural rubber composites eliminates the acid and salt flocculants. This reduction in the generation of waste gases and equipment corrosion during the flocculation process enhances the preparation quality of natural dry rubber. The research provides significant theoretical and practical implications for realizing high-quality natural dry rubber.

Graphical abstract

Keywords: silica; natural rubber; 8150; flocculation; rolling resistance

1 Introduction

Natural rubber latex (NRL), a polymer emulsion synthesized by the rubber tree through photosynthesis, primarily comprises rubber hydrocarbons, accompanied by proteins, fatty acids, sugars, and other non-rubber substances. Extraction from rubber trees yields natural rubber, a substance-free from the pollution issues associated with synthetic rubber synthesis. Natural rubber (NR) exhibits exceptional elasticity, fatigue resistance, and tensile strength, and serves as a crucial raw material in high-quality tire manufacturing (1,2,3). The surface of rubber particles in natural latex forms a protective layer through hydrophilic substances such as charged proteins and lipids, retaining the stable colloidal state of latex. Disruption or attenuation of this protective layer can result in latex destabilization and flocculation (4).

NR is derived through a process involving natural latex collection, flocculation, gel block cleaning, and drying. Among these, natural latex flocculation is a pivotal step. Various methods, such as adding acids, inorganic salts, or microorganisms and heating or freezing, can be employed to flocculate natural latex. The selected flocculation method influences the structure of NR, consequently impacting its performance. In China, the acid flocculation method is predominantly employed in NR production (5). Wititsuwannakul et al. (6) utilized natural coagulation for the flocculation of natural rubber, revealing that microbial action in the latex led to protein degradation, diminishing rubber particle stability and causing flocculation. This process retained a higher proportion of non-gelatin fractions in natural rubber, resulting in the formation of a dense network structure. Xiao et al. (7) incorporated potassium oleate into natural rubber latex and employed microwave flocculation and drying to produce natural dry rubber. Their findings indicated that this process resulted in a high plasticity retention rate, allowing for the incorporation of more non-rubber components, ultimately forming a robust vulcanization network structure. Consequently, the tensile strength of vulcanized rubber increased by 13.5%, and the aging retention rate improved by 15.3 times. In the 1960s, Sethulekshmi et al. (8) and others discovered that combining natural latex with metal salts such as Ca/Mg or Zn-containing strong bases and weak acid salts shortened flocculation time. Notably, the presence of divalent Ca2+ demonstrated the most significant advantage, enabling coagulation even in higher pH environments. However, the presence of metal ions remained detrimental to aging resistance. Traditionally, the standard natural rubber production process in China relies on acid coagulation of latex. Unfortunately, this method corrodes equipment, generates unpleasant odors, and releases acid-containing waste gas and wastewater. Additionally, it adversely affects natural rubber quality, resulting in subpar performance of standard natural rubber. Therefore, adopting an acid-free flocculation method for natural rubber preparation is imperative (9,10).

Silica, scientifically termed precipitated hydrated silica and prepared through organosilicates, is a non-toxic, odorless white powder with a low production cost. Due to its high specific surface area and excellent chemical inertia, it finds widespread application in chemical materials and various fields. With the depletion of non-renewable resources such as oil and natural gas, there is a need to explore environmentally friendly fillers as alternatives to traditional rubber fillers derived from petroleum. Silica exhibits a reinforcing effect on rubber akin to carbon black, effectively reducing tire rolling resistance and enhancing wet skid resistance. This makes it suitable for the production of eco-friendly tires, contributing to the reduction of carbon dioxide emissions, environmental preservation, and energy conservation (11,12,13,14). The surface of silica is abundant in hydroxyl groups, resulting in a pronounced adsorption agglomeration tendency. Moreover, its compatibility with non-polar natural rubber is suboptimal, and the acidic nature of the hydroxyl groups leads to the adsorption of vulcanization accelerators during the mixing process. This diminishes vulcanization efficiency, adversely affecting the crosslinking density of the rubber material (15). Consequently, silane coupling agents are commonly employed to modify silica, enhancing its bonding with rubber (16,17,18,19).

Crosile® 8150, an amino silane oligomer aqueous silane (hereafter referred to as 8150), is a colorless transparent liquid, functioning as a bifunctional organic compound with an alkaline pH. The silica hydroxyl group in 8150 can bond to inorganic substrates, and its amino group can interact with suitable organic polymers. Therefore, it serves as a silane coupling agent, improving dispersion when blended with silica to prepare composites. To address issues such as poor aging resistance of acid coagulation, environmental pollution, challenges in silica dispersion, and inadequate interfacial bonding between silica and rubber, this study employs 8150 flocculation to prepare natural rubber. Subsequently, composites with excellent mechanical properties and reduced rolling resistance are developed. 8150 serves as a green flocculating agent, fostering the formation of a more pliable raw rubber network through 8150 coagulation. This enhances silica compatibility with natural rubber and improves silica dispersion within the rubber matrix. The flexibility of molecular chains, plasticity retention rate, crosslinking density of raw rubber, vulcanization characteristics, mechanical properties, and dynamic mechanical properties of silica/NR composites were investigated. The aqueous silane flocculation process presented in this study addresses the drawbacks associated with acid flocculation, aligns with the principles of green environmental protection, and holds significant theoretical and practical implications for the preparation of high-quality natural raw rubber.

2 Materials and methods

2.1 Materials

Natural rubber latex (60% solids) was procured from Hainan Natural Rubber Industry Group Co., Ltd; Ribbed Smoked Sheet (RSS) was obtained from Hainan Natural Rubber Industry Group Co., Ltd; Silica 1165 was purchased from Solvay Silica (Qingdao) Co., Ltd; Silane coupling agent Si69, 8150, zinc oxide (ZnO), stearic acid (SAD), sulfur (S), and accelerator NS were all commercially available industrial-grade products.

2.2 Experimental formulation

NR 100; silica 1165 35; Si69 3; ZnO 5; SAD 2; S 2.25; accelerator NS 0.7. The RSS was named as group A, 2, 4, 6phr 8150 flocculated natural raw rubber was named as groups B, C, and D, respectively.

2.3 Experimental equipment

The experimental equipment and their manufacturer details are given in Table 1.

Table 1

Experimental equipment and manufacturer

Equipment Model Manufacturer
Electric blast drying oven DHC-9035A Shanghai Yiheng Technology Co.
Kneader X(C)K-160 Shanghai Double Wing Rubber Machinery Factory
Harp mixing torque vulcanizer RM-200C Harbin Harper Electric Technology Co.
Flatbed vulcanizing machine XLD-400 × 400 × 2 Qingdao Yilang Rubber Equipment Co.
Rubber dynamic processing analyzer RPA2000 American Alpha Technologies, Inc.
Rotorless rheometer MDR-C American Alpha Technologies, Inc.
Rubber hardness tester Wallace H17A Wallace & Sons UK
Rapid plasticity meter P14 Wallace & Sons UK
Universal Testing Machine Instron 3365 Instron USA, Inc.
DIN abrasion tester SS-5643-D China Taiwan Songshu Testing Instrument Co.
Nuclear magnetic resonance crosslink densitometer XLDS-15 HT MK5 IIC Dr KUHN GMBH & CO., Germany
Temperature scanning stress relaxation analyzer TSSR-Meter Brabender, Germany
Differential scanning calorimeter 214 NETZSCH, Germany
Dynamic thermomechanical analyzer EPLEXOR 150N GABO Company, Germany

2.4 Sample preparation

The flow of the preparation process is illustrated in Figure 1.

Figure 1 Flow of the preparation process.
Figure 1

Flow of the preparation process.

2.4.1 Preparation of natural raw rubber flocculated by 8150

A specific quantity of NRL was taken in a beaker, followed by the addition of a measured amount of 8150 (concentration of 40%) to the latex-containing beaker. The mixture was stirred, leading to the gradual solidification of NRL. 8150, containing amino acids and alkali substances, facilitated the hydrolysis of proteins in latex, interacting with low-grade fatty acids to form salts. This process induced protein denaturation, reduced hydration degree, and diminished the colloidal stability of the latex. Subsequently, the solidified rubber underwent dehydration in a twin-screw extruder at a temperature of 100°C and a rotational speed of 30 rpm.

Flocculation of NRL and 8150 in ratios of 100:2, 100:4, and 100:6 yielded 8150 flocculated natural raw rubber, denoted as 2phr8150, 4phr8150, and 6phr8150, respectively.

2.4.2 Mixing

A specific quantity of natural rubber (including RSS and 8150 flocculated natural raw rubber), silica, Si69, and other rubber additives were weighed according to the formula. First, press the natural rubber onto the roller of the open mill, then add it to the internal mill for 1.5 minutes of plasticization, and finally, add all rubber additives and silica. When the temperature reaches 145°C, keep warm and mix for 1 minute. The distance of the open mill was adjusted to the minimum, and the rubber discharged from the mixer was placed on the open mill rollers for a thin pass. The rubber on both sides of the knife was layered with S and NS until the surface was relatively smooth. The rubber material was then inserted vertically between the rollers, alternating between roll and triangular packages three times, after which the roller distance was increased for the thicker rubber compound.

2.4.3 Vulcanization

After being rested for 12 h, the rubber compound was tested using a rotorless rheometer and vulcanization according to 1.3t 90 based on the t 90 time of the rotorless test. The mixed rubber was molded for vulcanization on a plate vulcanizing machine under the condition of 150°C/10 MPa × 1.3t 90 to obtain vulcanized rubber.

2.5 Performance characterization

2.5.1 Differential scanning calorimetry (DSC)

An empty crucible serves as a reference. Approximately 5 mg of natural raw rubber was taken. The temperature was lowered from 10°C to −100°C at a cooling rate of 10 K·min−1, held for 10 min, and then heated from −100°C to 100°C at a heating rate of 20 K·min−1.

2.5.2 Plasticity initial value (P 0) and plasticity retention index (PRI)

P 0 and PRI were determined according to ISO 2007-1991 and ISO 2930-1995, respectively. The samples, plasticized by rollers, were cut into small disks of 3.2–3.6 mm. The P 0 and PRI were determined using a rapid plasticometer type P14 on seven unaged and seven aged specimens (heated in an electric blast drying oven at 140°C for 30 min). The PRI was calculated using the following equation:

P RI = P 30 P 0 × 1 00 %

where P 0 was the plasticity value of the unaged specimen, and P 30 was the plasticity value of the specimen after aging at 140°C for 30 min.

2.5.3 Nuclear magnetic resonance crosslink density (HNMR)

The German IICXLDS-15 HT MK5 nuclear magnetic resonance cross-linking densitometer was utilized to ascertain the cross-linking density of raw rubber. The measurements were conducted with a magnetic induction intensity of 315 A·m−1, a frequency of 15 MHz, and a controlled test temperature of 80°C.

2.5.4 Payne effect

A rubber processing analyzer was employed to test the Payne effect of the rubber. The strain range spanned from 0.28% to 40%, and the frequency was set at 0.01 Hz.

2.5.5 Temperature scanning for stress relaxation (TSSR)

TSSR tests were executed using a Brabender Temperature Scanning Stress Relaxer from Germany. The small dumbbell-shaped samples were used according to ASTM G154-05. Initially, a constant tensile strain of 50% was applied to the specimens. After the completion of the tensile force, the samples underwent isothermal relaxation at 25°C for 2 h. Subsequently, the samples were heated to 300°C at a rate of 2°C·min−1 until stress relaxation was realized.

2.5.6 Vulcanization characteristics

The vulcanization characteristics of the rubber composites were assessed using a rotorless rheometer, following the standard (ISO 6502-2: 2018) test. The test temperature was set at 150°C.

2.5.7 Mechanical properties

The hardness of the vulcanizate was measured using the Shore A Hardness Tester by the standard (ISO 7619-2: 2004). The tensile properties of vulcanized adhesives were tested using a tensile testing machine, following the standards (ISO 37: 2005 and ISO 34-1: 2004).

2.5.8 Dynamic mechanical properties

The dynamic mechanical properties of vulcanized rubber were examined with a dynamic thermomechanical analyzer. The dynamic stress was 60 N, dynamic strain was 0.25%, static stress was 70 N, static stress was 5%, heating rate was 2°C·min−1, temperature range was from −65°C to 65°C, and frequency was 10 Hz.

3 Results and discussion

3.1 DSC

The glass transition temperature, denoted as T g, signifies the temperature at which a polymer transitions from a highly elastic state to a glassy state. It represents the lowest temperature at which segments of the amorphous polymer macromolecular chain can freely move. This temperature is critical, defining the boundary between elasticity and brittleness in polymers. For rubber materials, operating at temperatures below the T g renders them glassy and rigid, jeopardizing elasticity and causing them to become brittle and hard. This can lead to the failure of rubber products, impacting production and utility (20). The molecular flexibility, inversely proportional to T g, increases with a more flexible molecular chain, providing greater free volume during molecular chain rotation. DSC is a widely employed technique for measuring thermal transformations, including crystallization and glass transition, in polymers. Figure 2 presents the DSC curves and T g of the natural raw rubbers. The T g for the four raw natural rubbers are observed to be −58.7°C, −59°C, −59.3°C, and −60.9°C, respectively. Notably, the T g for 8150 flocculated natural raw rubber is generally lower compared to the RSS, indicating improved molecular flexibility. The addition of acid during the flocculation of RSS intensifies molecular chain oxidation and breakage, resulting in reduced flexibility.

Figure 2 (a) DSC curve and (b) glass transition temperature (T g).
Figure 2

(a) DSC curve and (b) glass transition temperature (T g).

3.2 HNMR

Kuhn et al. (21,22) investigated the network structure and crosslink density of vulcanized rubber using NMR spectroscopy. They concluded that the crosslink density determined by the NMR method correlates well with that determined by the conventional method, establishing a relationship between HNMR relaxation parameters and the structure of vulcanized rubber (23). Table 2 displays the 1H-NMR relaxation parameters of RSS and 8150 flocculated natural raw rubber. According to Kuhn’s theory, the crosslink density of unvulcanized rubber primarily constitutes the physical crosslink density, characterized by physical entanglement points. As indicated by the data in Table 2, 8150 flocculated natural raw rubber exhibits a lower total crosslink density compared to RSS. This discrepancy arises from the acid flocculation of RSS, resulting in pronounced chain breakage, shorter molecular chains, and a heightened entanglement phenomenon, consequently leading to a higher total crosslink density. With an increase in 8150 content, the crosslink density initially rises and then diminishes. Mc, denoting the average relative molecular mass of the chains between cross-linking sites, typically decreases with a higher crosslinking density. The transverse relaxation time (t 2) signifies the duration for the magnetic field intensity to decay to 36.79% of the total intensity. It reflects intramolecular dipole interactions among the carbon chain protons and relates to the molecular motions of the entire network, encompassing both fast motions of small molecules, free ends, and free molecules, as well as relatively slower web-chain motions and the slowest motion of the entire network. A shorter relaxation time suggests more restricted molecular motion (24). Table 2 reveals that the relaxation time t 2 of 8150 flocculated natural raw rubber is typically shorter than that of RSS. This phenomenon may be attributed to the substantial energy required to disrupt 8150 flocculated raw rubber, making the cross-linking points resistant to destruction. Consequently, molecular movement is more restricted, resulting in a shorter relaxation time t 2.

Table 2

1H-NMR relaxation parameters of RSS and 8150 flocculated natural raw gums

Relaxation parameter RSS 2phr8150 4phr8150 6phr8150
Total crosslink density × 10−5/(mol·cm−3) 27.96 ± 5.56 5.82 ± 0.00 6.04 ± 0.00 5.68 ± 0.00
Average relative molecular mass Mc (kg·mol−1) 3.18 ± 0.63 14.95 ± 0.01 14.41 ± 0.01 15.32 ± 0.01
Relaxation time t 2/ms 2.82 ± 0.12 2.70 ± 0.11 2.65 ± 0.11 2.63 ± 0.09

3.3 Plasticity retention

The PRI serves as a crucial indicator, reflecting the antioxidant and high-temperature operational performance of raw rubber. This index, denoted as PRI, represents the percentage ratio of the plasticity value (P 30) to the initial plasticity value (P 0) after the raw rubber undergoes heat treatment at 140°C for 30 min. Consequently, it is also referred to as the antioxidant index. Rubber plasticity, a pivotal metric for identifying rubber quality, significantly impacts rubber processing technology and product quality (25). As depicted in Figure 3, the P 0 of 8150-flocculated natural raw rubber aligns closely with that of RSS, and consistently maintained within a specific range. In comparison to RSS, the PRI of 2, 4, and 6 phr 8150-flocculated natural raw rubber exhibits improvements, registering increments of 18.32%, 1.75%, and 22.18%, respectively. Remarkably, the PRI of 6 phr 8150-flocculated natural raw rubber is the highest (102.29%). This enhancement can be attributed to the acid flocculation-induced oxidized chain breakage in RSS, leading to an unfavorable acid residue that compromises aging resistance. Building upon the findings from DSC and HNMR, the 8150 flocculation process adeptly preserves the integrity and flexibility of molecular chains during flocculation. Despite the lower cross-link density, the 8150-flocculated raw rubber establishes a more flexible and robust network. This augmentation fortifies the molecular chain’s resistance against hot air-induced deterioration in the PRI test, subsequently enhancing the aging resistance of the raw rubber. The effect of acid coagulation and the 8150 coagulation process on the molecular chain is illustrated in Figure 4.

Figure 3 Plasticity initial value P 0 and plasticity retention rate PRI.
Figure 3

Plasticity initial value P 0 and plasticity retention rate PRI.

Figure 4 Crosslink densities of RSS and 8150 flocculated natural raw rubber.
Figure 4

Crosslink densities of RSS and 8150 flocculated natural raw rubber.

3.4 Payne effect

Figure 5(a) illustrates the energy storage modulus curve of the compounded rubber concerning strain. The phenomenon of the energy storage modulus of a filler-filled rubber diminishing with increasing strain is recognized as the Payne effect (26). ΔG′ denotes the degree of network structuring of the filler, where a smaller ΔG′ corresponds to a weaker filler-filler network structure, indicating a milder Payne effect and improved rubber processability (27). The Payne effect is intricately linked to the disruption of the filler network, the interaction between polymer chains and fillers, and the entanglement between polymer chains (28). As indicated by Figure 5, the Payne effect of 2, 4, and 6 phr 8150/NR compound is notably reduced compared to RSS, registering reductions of 35.87%, 41.81%, and 1.35%, respectively. Among these, 4 phr 8150/NR composite exhibits the lowest Payne effect with ΔG′ measuring 79.11 kPa. This reduction can be attributed to the robust bonding between the filler and rubber in the 8150/NR composites, resulting in an enhanced filler-rubber network structure. Consequently, the Payne effect diminishes, contributing to improved processability.

Figure 5 (a) Variation in the energy storage modulus of the compound with strain and (b) changes in the energy storage modulus.
Figure 5

(a) Variation in the energy storage modulus of the compound with strain and (b) changes in the energy storage modulus.

3.5 TSSR

Figure 6 illustrates the Tx and crosslink density as measured by TSSR. T10, T50, and T90 represent temperatures at 10%, 50%, and 90% stress reduction, respectively, with T90 presumed as the sample’s failure temperature. The T90 for RSS (vulcanized rubber) stands at 180.4°C, while the 2, 4, and 6 phr 8150/NR vulcanized rubber show values around 193°C, marking increments of 7.31%, 6.98%, and 7.15%, respectively. This suggests that the inclusion of 8150 enhances the heat-resistant stability of the rubber composite materials. As depicted in Figure 6(b), vulcanized rubber containing 8150 generally exhibits a higher crosslink density compared to that of RSS. The crosslink density of RSS (vulcanized rubber) and 8150 vulcanized rubber is 96.62, 132.85, 115.25, and 123.13 mol·m−3, respectively. The crosslink density of 8150 vulcanized rubber increases by 37.49%, 19.28%, and 27.43%, respectively, compared to RSS (vulcanized rubber). This increase is attributed to the effective dispersion of the filler in 8150 vulcanized rubbers, resulting in improved bonding between the filler and rubber. The original bonding ability between rubber molecular chains is preserved, making it resistant to destruction and leading to a higher cross-linking density in 8150 vulcanized rubber. Despite the high crosslink density in acid-solidified raw rubber (RSS), poor flexibility of the molecular chain results in insufficient dispersion of silica in the rubber matrix, making the crosslink density of 8150 vulcanized rubber greater than that of RSS (vulcanized rubber).

Figure 6 (a) T10, T50, and T90 and (b) crosslink density of four natural rubber composites.
Figure 6

(a) T10, T50, and T90 and (b) crosslink density of four natural rubber composites.

3.6 Vulcanization characteristics

The vulcanization characteristics of RSS (vulcanized rubber) and 8150 vulcanized rubber are presented in Table 3. M L characterizes the fluidity of the rubber composite, with a smaller M L indicating better fluidity. t 10 denotes the time required for 10% vulcanization, known as the safe processing time for the rubber material. t 90 represents the time required for 90% vulcanization, signifying the positive process vulcanization time. A shorter t 90 implies a more efficient process and a better economy. As indicated by the data in Table 3, the M L of 8150-flocculated vulcanized rubber is larger than that of RSS vulcanized rubber. This may be attributed to the effective dispersion of the filler in 8150-flocculated vulcanized rubber, leading to a reduction in fluidity. The t 10 and t 90 of 8150-flocculated vulcanized rubber are lower than those of RSS vulcanized rubber, with shorter processing times indicating improved vulcanization efficiency. The weak alkalinity of 8150-flocculated vulcanized rubber promotes vulcanization, and its well-dispersed nature contributes to a more perfect crosslinking network in the rubber composites, facilitating vulcanization.

Table 3

Vulcanization characteristics

RSS 2phr8150 4phr8150 6phr8150
M L/(dN·m) 1.68 1.99 1.79 2.03
M H/(dN·m) 13.19 12.34 12.08 12.29
t 10/min 6.63 3.92 2.62 1.85
t 90/min 25.97 17.92 13.96 11.59

3.7 Mechanical properties

As indicated by Figure 7(a), the tensile strength and hardness of 8150 vulcanized rubber surpass those of RSS (vulcanized rubber). The tensile strength increases by 17.57%, 16.70%, and 29.34%, respectively. As illustrated in Figure 7(b), the 100% constant tensile stress and 300% constant tensile stress of 8150 vulcanized rubber are generally higher than those of RSS (vulcanized rubber). The 100% constant tensile stress increases by 31.57%, 37.71%, and 35.96%, while the 300% constant tensile stress rises by 61.09%, 94.17%, and 91.54%, respectively. Figure 7(c) indicates that the tensile product of 8150 vulcanized rubber is generally higher than that of RSS (vulcanized rubber), with the most significant enhancement observed in 6phr 8150 vulcanized rubber at 13.04%. Due to the increased constant tensile stress, the corresponding elongation at break decreases. The effective combination between the filler and rubber in 8150 vulcanized rubber results in a stronger bond, reducing the likelihood of slip and friction between the filler and rubber. Additionally, the dense three-dimensional network structure formed by the high crosslinking density alleviates stress concentration, contributing to the enhancement of mechanical properties.

Figure 7 (a) Tensile strength and hardness, (b) tensile stress at 100% and 300% elongation, (c) elongation at break and tensile product, (d) resilience and abrasion.
Figure 7

(a) Tensile strength and hardness, (b) tensile stress at 100% and 300% elongation, (c) elongation at break and tensile product, (d) resilience and abrasion.

Compared with RSS (vulcanized rubber), 8150 vulcanized rubber exhibits 18.73%, 16.10%, and 21.80% lower abrasion volume, respectively. The inferior abrasion resistance of vulcanized rubber containing RSS is attributed to poor filler dispersion and elevated heat generation during wear, resulting in material softening and reduced abrasion resistance (29). As shown in Figure 7(d), the resilience properties of 8150 vulcanized rubber generally surpass those of RSS (vulcanized rubber), with resilience values increasing by 7.5%, 8.6%, and 9.8%, respectively.

3.8 Dynamic mechanical properties

Figure 8 illustrates the dynamic mechanical properties of vulcanized rubber, with Figure 8(b) and (c) offering detailed views of Figure 8(a). In Figure 8(a), the loss factor (Tanδ) of vulcanized rubber in the range of −65°C to 65°C is presented. Tanδ, known as the loss factor, is associated with energy loss and indirectly characterizes wet skid resistance and rolling resistance. The Tanδ near 0°C characterizes the wet skid resistance of tires, with a larger Tanδ indicating superior wet skid resistance. Conversely, the Tanδ near 60°C characterizes the rolling resistance of tires, with a smaller Tanδ indicating lower rolling resistance (30,31,32). Figure 8(b) and (c) reveal significantly reduced Tanδ values for 8150 vulcanized rubber at 0°C and 60°C, with 6phr 8150 displaying the lowest Tanδ value, signifying the best rolling resistance. Table 4 further indicates a 34.05%, 39.16%, and 47.21% reduction in rolling resistance for 8150 vulcanized rubber compared to RSS (vulcanized rubber), respectively. This is attributed to the superior interfacial bonding between filler and rubber and the high bonding strength of entanglement points between rubber molecules, leading to reduced sliding or damage between rubber molecular chains or between rubber and filler and less energy loss. Consequently, the Tanδ is smaller, resulting in reduced rolling resistance.

Figure 8 (a) Dynamic mechanical property curves, (b) localized magnification at 0°C, and (c) localized magnification at 60°C.
Figure 8

(a) Dynamic mechanical property curves, (b) localized magnification at 0°C, and (c) localized magnification at 60°C.

Table 4

Relationship between the loss factor and temperature

RSS 2phr8150 4phr8150 6phr8150
Tanδ (0°C) 0.1370 0.1165 0.1072 0.1013
Tanδ (60°C) 0.0881 0.0581 0.0536 0.0465

4 Conclusion

In this study, natural rubber composites were prepared using various proportions of 8150 flocculation, gaining insights for enhancing silica-reinforced natural rubber. The experimental findings indicated that the natural rubber prepared through 8150 flocculation exhibited a more refined network structure, exhibiting superior overall performance. The PRI for natural raw rubber flocculated with 2, 4, and 6 phr 8150 improved by 18.32%, 1.75%, and 22.18%, respectively, compared with RSS. Compared to the RSS composites, the silica/natural rubber composites prepared with 4phr8150 showed 41.81%, 39.16%, and 16.1% reduction in Payne effect, rolling resistance, and abrasion volume, respectively, and 16.7%, 94.17%, and 19.28% increase in tensile strength, tensile stress at 300% elongation and crosslinking density, respectively. The poorer the rolling resistance, the higher the hysteresis loss and heat generation, so the 8150 flocculated NR had low heat generation. The 8150 flocculation of NR composites eliminates the need for acid and salt flocculants, thereby reducing the emission of waste gases during the flocculation process. This not only enhances the quality and efficiency of the preparation of natural dry rubber but also holds significant theoretical and practical implications for producing high-quality natural dry rubber.

  1. Funding information: This research was supported by National Natural Science Foundation of China (52173101) and Natural Science Foundation of Shandong Province (ZR2020KE037).

  2. Author contributions: Pengfei Diao: methodology, investigation, data curation, and writing – original draft; Yao Xiao: investigation and formal analysis; Zheng Gong: investigation and formal analysis; Shenglong Yang: visualization; He Wang: investigation; Chuansheng Wang: resources and methodology; Huiguang Bian: conceptualization and methodology.

  3. Conflict of interest: The authors declare no conflict of interest.

  4. Data availability statement: Data will be made available on request.

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Received: 2024-02-29
Revised: 2024-04-24
Accepted: 2024-04-24
Published Online: 2024-12-31

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/epoly-2024-0029
Keywords for this article
silica; natural rubber; 8150; flocculation; rolling resistance
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Flame-retardant thermoelectric responsive coating based on poly(3,4-ethylenedioxythiphene) modified metal–organic frameworks
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  59. Experimental investigation on low-velocity-impact and post-impact-tension behaviors of GFRP T-joints after hydrothermal aging
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  74. Development of smart core–shell nanoparticles-based sensors for diagnostics of salivary alpha-amylase in biomedical and forensics
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