Effect of Wet Mixing on Properties of Radial-Orientation Basalt Fiber-Reinforced Rubber Compounds
Abstract
:1. Introduction
2. Materials and Methods
2.1. Raw Material
2.2. Experimental Equipment
2.3. Preparation Experiments of Short-Fiber-Reinforced Composites
2.3.1. Preparation Experiments and Delay Formulation Mechanism of Different Types of Short-Fiber-Reinforced Composites
- (1)
- (a) First-stage mixing: we lifted the top bolt, put the NR cut into small pieces into the mixer from the feeding port, closed the top bolt, adjusted the rotor speed to 70 r/min, and mixed for 30 s. We then lifted the top bolt, added 8 phr silica, 22.5 phr carbon black N234, 1 phr Si 69 and 3 phr BF, closed the top bolt, and mixed for 120 s; 70 r/min.We then lifted the top bolt, added 3.5 phr ZnO, 2 phr stearic acid, 1 phr microcrystalline wax, 22.5 phr carbon black, 1.5 phr antioxidant RD, 1.5 phr 4020, 1.6 phr NS and 0.08 phr of plasticizer, closed the top bolt, adjusted the rotor speed to 40 r/min, and mixed for 4 min and 30 s.(b) Second-stage mixing: We added 1 phr sulfur to the master batch obtained in step (a), mixed for 1 min, and discharged the compound.
- (2)
- After the mixing was uniform, the sheet was opened, and the obtained rubber was calendered and oriented along the short-fiber direction. The specific method was as follows:
- (1)
- The raw materials were proportioned and weighed, and sequentially added to an internal mixer for mixing.
- (1)
- Firstly, the natural latex was subjected to wall-breaking treatment, and 850 g natural latex (60% by mass) solution was stirred in a high-speed mixer at 1800 r/min for 8 min;
- (2)
- We took the silane coupling agent KH560, 1.5 g/L, 40 mL, and added it into a 850 g natural latex (60% by mass) solution, and stirred it at 1800 r/min in a high-speed mixer for 1 min;
- (3)
- We cleaned a proper amount of BFs with deionized water (treated with KH550), added BF to the treated natural latex after the water was clear, stirred for 1 min at 1800 r/min under normal temperature, poured it into a glass dish after completion, and dried it in an oven for 6 h; cut into small pieces, the NR/BF masterbatch was prepared.
- (1)
- Firstly, the natural latex was subjected to wall-breaking treatment, and 850 g natural latex (60% by mass) solution was stirred in a high-speed mixer at 1800 r/min for 8 min;
- (2)
- We washed 3 phr BF with deionized water (treated with KH550). After the water was clear, we put 3 phr BF into 40 mL of 1.5 g/L KH560 solution with equal concentration, and heated it in water bath for 2 h. The coupling agent KH560 was attached to the surface of the fibers; it was taken out and placed in the oven for 4 h of drying;
- (3)
- We took out the BF after BF drying, added the BF to the treated natural latex, stirred it at 1800 r/min for 1 min under normal temperature, poured it into the glass dish after completion, and dried it in the oven for 6 h; cut into small pieces, the NR/BF masterbatch was prepared.
- (1)
- Firstly, the natural latex was subjected to wall-breaking treatment, and 850 g natural latex (60% by mass) solution was stirred in a high-speed mixer at 1800 r/min for 8 min;
- (2)
- We took silane coupling agent KH560, 1.5 g/L, 40 mL, and added it to the 850 g natural latex (60% by mass) solution, and stirred it at 1800 r/min in a high-speed mixer for 1 min. We then washed a proper number of BFs with deionized water (treated with KH550), added 3 phr BF to the treated natural latex after the water was clear, and stirred at 1800 r/min for 1 min under normal temperature;
- (3)
- We weighed 258 g carbon black (N234) and put it into a beaker, then poured 800 g deionized water. Then, we stirred the carbon black aqueous solution in a stirrer with a stirring speed of 750 r/min and a stirring time of 5 min to fully dissolve the carbon black;
- (4)
- Then, the latex was poured into the carbon black aqueous solution (poured while stirring); the stirring speed was 750 r/min, and the stirring time was 1 min. After completion, it was poured into the glass dish, dried in the oven for 6 h, and then poured into the large tray to be laid and dried to prepare the NR/BF masterbatch.
- (a)
- We adjusted the bar pitch of the open mill to 1 mm, and rolled the roll 5 times along the rolling direction of the open mill. Then, we adjusted the pitch to 3 mm, and paid close attention to passing the roller 5 times along the rolling direction to obtain the short-fiber-reinforced compounds with the most fibers oriented along the rolling direction;
- (b)
- At the end of vulcanization, the performance test should be carried out, and the compounds should be stored for 24 h for standby; this is conducive to the uniformity and stability of the compounds’ properties and the relaxation of the internal stress of the rubber macromolecule.
2.3.2. Extrusion Experiment of Different Compounds and 3D Physical Model of Extruder Die
2.4. Characterization
2.4.1. Physical and Mechanical Property Test and Wear Resistance
Preparation of the Test Sample
Performance Test
2.4.2. SEM Scanning Test Process
2.4.3. Payne Effect
2.4.4. Mooney Test Process
2.4.5. Dynamic Thermomechanical Analysis
2.4.6. Hardness
2.4.7. Three-Dimensional Topography Test
2.4.8. Carbon Black Dispersion Meter Test
3. Analysis and Discussion of Test Results
3.1. Vulcanizate in Filler System, Vulcanization Performance, Physical and Mechanical Properties and Dispersion Effect, SEM Analysis
3.1.1. Vulcanization Performance Analysis
3.1.2. Physical and Mechanical Properties
3.1.3. SEM Analysis
3.1.4. Three-Dimensional Topography Test
3.1.5. BF on Dynamic Viscoelasticity of Composites
3.1.6. BF on Payne Effect of Composites
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Delayed Formula | Formulation (phr) | All-Steel Tire Formula | Formulation (phr) |
---|---|---|---|
NR | 85 | NR | 100 |
BR | 15 | Plasticizer | 0.08 |
Carbon black N234 | 43 | Carbon black N234 | 45 |
ZnO | 4 | ZnO | 3.5 |
SAD | 2 | SAD | 2 |
4020 | 2 | 4020 | 1.5 |
Microcrystalline wax | 1 | Microcrystalline wax | 1 |
S | 1 | S | 1 |
DZ | 1.8 | NS | 1.6 |
CTP | 0.3 | RD | 1.5 |
RD | 1 | Si69 | 1 |
Si69SiO2 | 0.55 | SiO2 | 8 |
Items | 1# | 2# | 3# | 4# | 5# | 6# | 7# |
---|---|---|---|---|---|---|---|
t10/min | 2.34 | 5.42 | 6.31 | 5.73 | 4.34 | 4.09 | 3.00 |
t90/min | 7.99 | 16.61 | 16.41 | 15.23 | 13.09 | 13.33 | 10.67 |
ML/(dN·m) | 3.50 | 3.08 | 3.33 | 2.91 | 3.88 | 4.19 | 3.09 |
MH/(dN·m) | 15.81 | 14.51 | 12.88 | 12.37 | 16.24 | 16.69 | 13.31 |
(MH-ML)/(dN·m) | 12.31 | 11.43 | 9.55 | 9.46 | 12.36 | 12.5 | 10.22 |
Mooney ML (1 + 4) | 76.25 | 76.73 | 78.65 | 74.43 | 87.57 | 97.09 | 77.99 |
Items | 1# | 2# | 3# | 4# | 5# | 6# | 7# |
---|---|---|---|---|---|---|---|
t10/min | 1.87 | 3.55 | 4.55 | 3.70 | 3.92 | 4.31 | 0.93 |
t90/min | 6.95 | 13.71 | 13.92 | 13.42 | 11.24 | 12.55 | 7.59 |
ML/(dN·m) | 2.79 | 2.40 | 2.63 | 2.18 | 3.16 | 3.31 | 2.59 |
MH/(dN·m) | 14.42 | 12.82 | 12.55 | 12.92 | 15.12 | 15.48 | 10.65 |
(MH-ML)/(dN·m) | 11.63 | 10.42 | 9.92 | 10.74 | 11.96 | 11.17 | 8.06 |
Mooney ML (1 + 4) | 73.14 | 73.95 | 74.43 | 66.52 | 85.28 | 94.11 | 74.96 |
Items | 1# | 2# | 3# | 4# | 5# | 6# | 7# |
---|---|---|---|---|---|---|---|
Hardness | 62 | 67 | 65 | 67.5 | 68.5 | 67.5 | 66 |
σ1 | 2.43 | 1.41 | 1.28 | 0.87 | 1.49 | 2.60 | 1.41 |
σ2 | 19.05 | 19.41 | 19.72 | 19.82 | 21.42 | 20.70 | 21.61 |
εt | 460.8 | 570.4 | 604.6 | 543.0 | 634.3 | 468.9 | 615.7 |
τt | 92 | 81 | 71 | 83 | 88 | 84 | 85 |
△V | 153.68 | 161.51 | 132.92 | 119.70 | 111.38 | 116.51 | 106.83 |
Mooney | 76.25 | 76.73 | 78.65 | 74.43 | 87.57 | 97.09 | 81.68 |
Carbon black dispersion | 5.43 | 6.25 | 6.12 | 6.83 | 6.20 | 6.36 | 6.91 |
Items | 1# | 2# | 3# | 4# | 5# | 6# | 7# |
---|---|---|---|---|---|---|---|
Hardness | 66 | 62.5 | 64 | 62.5 | 67 | 67 | 64 |
σ1 | 2.35 | 1.25 | 1.56 | 1.63 | 3.01 | 1.81 | 1.41 |
σ2 | 20.99 | 18.59 | 19.75 | 20.58 | 22.32 | 21.09 | 22.79 |
εt | 511.6 | 555.8 | 545.5 | 543.0 | 520.7 | 508.4 | 538.8 |
τt | 90 | 84 | 79 | 87 | 83 | 86 | 86 |
△V | 141.62 | 156.55 | 127.90 | 112.74 | 101.26 | 106.93 | 97.77 |
Mooney | 73.14 | 73.95 | 74.43 | 66.52 | 85.28 | 94.11 | 77.99 |
Carbon black dispersion | 7.51 | 7.36 | 7.50 | 7.97 | 7.00 | 7.25 | 7.98 |
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Yu, B.; Wang, J.; Wang, K.; Han, D.; Ren, J.; Zhang, D.; Wang, C. Effect of Wet Mixing on Properties of Radial-Orientation Basalt Fiber-Reinforced Rubber Compounds. Polymers 2022, 14, 4422. https://doi.org/10.3390/polym14204422
Yu B, Wang J, Wang K, Han D, Ren J, Zhang D, Wang C. Effect of Wet Mixing on Properties of Radial-Orientation Basalt Fiber-Reinforced Rubber Compounds. Polymers. 2022; 14(20):4422. https://doi.org/10.3390/polym14204422
Chicago/Turabian StyleYu, Benhui, Jing Wang, Kongshuo Wang, Deshang Han, Jianbin Ren, Dewei Zhang, and Chuansheng Wang. 2022. "Effect of Wet Mixing on Properties of Radial-Orientation Basalt Fiber-Reinforced Rubber Compounds" Polymers 14, no. 20: 4422. https://doi.org/10.3390/polym14204422
APA StyleYu, B., Wang, J., Wang, K., Han, D., Ren, J., Zhang, D., & Wang, C. (2022). Effect of Wet Mixing on Properties of Radial-Orientation Basalt Fiber-Reinforced Rubber Compounds. Polymers, 14(20), 4422. https://doi.org/10.3390/polym14204422