Extraction of microcrystalline cellulose from cotton fiber, and application to block natural rubber as reinforcing agent

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This paper reports on the extraction of microcrystal cellulose from cotton fiber and their application as a reinforcing agent in NR matrix. Microcrystalline cellulose was also grafted with maleic anhydride (MA) so that grafted one can improve interfacial interaction between cellulose and natural rubber. Fillers were incorporated to block natural rubber by two-roll mill dry mixing.

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Nội dung Text: Extraction of microcrystalline cellulose from cotton fiber, and application to block natural rubber as reinforcing agent

Cite this paper: Vietnam J. Chem., 2023, 61(S2), 73-80 Research Article DOI: 10.1002/vjch.202300070 Extraction of microcrystalline cellulose from cotton fiber, and application to block natural rubber as reinforcing agent Nguyen Ngoc An*, Pham Thi Le Chi Faculty of Chemistry, University of Science, Vietnam National University Ho Chi Minh City, 227 Nguyen Van Cu Street, District 5, Ho Chi Minh City 70000, Viet Nam Submitted February 19, 2023; Revised April 9, 2023; Accepted June 26, 2023 Abstract Crosslinked natural rubber (NR)/microcrystalline cellulose (MCC) composite was prepared by dry mixing of NR with MCC extracted from cotton fiber. MCC was first extracted from cotton fiber by acid hydrolysis processing, then applied to block natural rubber as a reinforcement. MCC grafted maleic anhydride (MA) was also synthesized and applied to the composites to improve the compatibility between natural rubber and cellulose. Obtained cellulose samples were subjected to infrared spectroscopy (FTIR) to confirm the purity of cellulose structure and the presence of MA grafted on MCC chains. X-ray spectroscopy (XRD) and thermogravimetric analysis (TGA) were investigated as well to see if there was any important change after modification. NR containing microcrystalline cellulose was formulated with vulcanizing agents and microcrystalline cellulose grafted MA for characterization. Micro-scale dispersion of microcrystalline cellulose was observed by scanning electron microscopy (SEM). MCC showed positive contributions to tensile strength and thermal properties of composites as well. Mechanical properties of vulcanized rubber containing microcrystalline cellulose grafted MA gave a slightly better value compared to the reference sample without adding the compatible agent. The presence of reinforcements helped NR composites to reduce solvent uptake, however there was no change in tensile strength after aging test. Keywords. Natural rubber, microcellulosse, composite, microcellulose grafted MA. 1. INTRODUCTION looking for through the years.[5-9] Microcrystalline cellulose (MCC) and nano Rubber is a very well-known natural elastic material, cellulose are considered the top bio-reinforcements in a polymer of isoprene, it means this polymer contains rubber composites due to their availability, natural unsaturated bonds in polymer chains which can be origin, and very promising mechanical connected to each other by cross-linking process or properties.[10,11] Microcrystalline cellulose (MCC) vulcanization. The vulcanization step will change can be extracted from various plants around the world: completely mechanical properties such as elasticity, palm trees, sisal bamboo, etc. even from the waste of abrasion resistance, elongation, tensile strength and agricultural products. This committee a stable tear strength, etc. of natural rubber. Then, they can be sourcing of natural, and low-cost fillers to be used in presented in various industrial sections from footwear rubber composite. However, cellulosic materials are and household product to very important presence in hydrophilic fillers while rubber is hydrophobic which transportation (tires), biomedical application as is completely un-compatible with each other. gloves, or others.[1-4] However, rubber needs fillers to Therefore, fillers dispersion in the rubber matrix reach a higher mechanical properties level for many should be improved and/or some modifications need industrial applications.[1,2] to be applied to these fillers to generate good One of the most important fillers for natural compatibility with the rubber matrix.[1,2,10] rubber is carbon black, thanks to the excellent This paper reports on the extraction of interfacial interaction between the CB particles and microcrystal cellulose from cotton fiber and their rubber chains. However, CB is a petroleum-based application as a reinforcing agent in NR matrix. material, non-biodegradable. Additionally, serious air Microcrystalline cellulose was also grafted with pollution and high energy consumption when CB is maleic anhydride (MA) so that grafted one can dispersed in a rubber matrix during mastication, so an improve interfacial interaction between cellulose and alternative bio-reinforcing agent for rubber has been natural rubber. Fillers were incorporated to block 73 Wiley Online Library © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH
25728288, 2023, S2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300070 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Nguyen Ngoc An et al. natural rubber by two-roll mill dry mixing. W= 98𝐶(𝑉0 − 𝑉1 ) × 100% 1000 ×2𝑚 2. MATERIALS AND METHODS 162W DS = 98 ×(100−W) 2.1. Materials where W is the content of maleic anhydride substituted, %. m is the mass of the sample, g. C is the NR was supplied by Phu Rieng rubber company, concentration of aqueous hydrochloric acid solution, Vietnam. Cotton fiber was purchased from Bong mol/L. V0 is the consumed volume of aqueous Bach Tuyet Company, Vietnam, and was used for hydrochloric acid solution by reference sample, mL. extraction of microcrystalline cellulose. H2SO4 98% V1 is the consumed volume of aqueous hydrochloric (China), NaOH (China), maleic anhydride (Aldrich), acid solution by esterified cellulose sample, mL. xylene (Aldrich). Dialysis membrane (Bio Basic, Canada, 44 mm, molecular cutoff 14,000 Daltone) 2.4. Compounding 2.2. Extraction of microcrystalline cellulose In this step, the NR/MCC composite was carried out using a two-roll mixing-mill. The formulations used Microcrystalline cellulose was prepared by acid are given in table 1. There are 2 series, MCC was hydrolysis of cotton fiber. Small size cotton fibers (2 mixed directly with NR at 1, 3, 5 and 7% in weight of cm) were treated with 35% H2SO4 at 1:12 (g/mL) dry rubber in one series, sample nominations were ratio. The suspension was heated at 50oC for 2.5 h. fixed as NR-M1, NR-M3, NR-M5 and NR-M7 After reaction, the product was washed with distilled accordingly. And the second series of fillers which water several times until a stable pH between 6.8-7.2. compose of 90% of MCC and 10% of Excess acid was removed by repeated centrifugation in Microcrystalline cellulose grafted MA were also distilled water at 12000 rpm for 10 minutes, and applied at 1, 3, 5 and 7% in weight of dry rubber. This obtained slurry was finally vacuum-dried at 60oC for 24 series includes NR-Mg1, NR-Mg3, NR-Mg5 and NR- h. The detail processing and resultats have been Mg7 respectively. Pure natural rubber was prepared presented in previous work.[11] in the same condition as well for reference. Vulcanization was carried out at 150oC for 10 mins. 2.3. Maleic anhydride (MA) grafted onto microcrystalline cellulose (MCC-g-MA) Table 1: Composite formulation Dissolving of 50.00 g maleic anhydride (MA) in 60.0 Ingredients Amount (prh) mL xylene, then 10.00 g MCC was added. The Natural rubber 100 grafting process was carried out at 80oC under stirring Zinc oxide (ZnO) 5 in the atmosphere of N2. After 3h of reaction, the Stearic acid 2 sample was washed several times with distilled water and a dialysis membrane filter was applied to remove Sulfur 2 excess MA. Vacuum drying of MCC-g-MA was CBS 1 carried out at 60°C for 24 h. MCC 1, 3, 5, 7% in weight NR MCC:MCC-g-MA 1, 3, 5, 7% in weight NR Determination of degree of substitution (DS) (9:1) The degree of substitution of the maleylation celluloses was determined by the back-titration 2.5. Experimental methods method.[12,13] 1.00 g of dry maleated cellulose was dissolved in 10.00 mL of 75% ethanol solution in The equipment used for FTIR investigation is a deionized water, and 10.00 ml of 0.5 M aqueous PerkinElmer MIR/NIR Frontier machine sodium hydroxide solution. The solution was stirred (PerkinElmer, USA). The palleted sample was during 30 min at room temperature until the solution scanned with wave number ranging from 4000 to 400 was homogeneous and transparent. The excess alkali cm−1. X-ray diffraction (XRD) was performed on a was back-titrated by 0.5 M aqueous hydrochloric acid PANalytical X'pert 3 Powder diffractometer solution, using Phenolphthalein as an indicator. DS (PANalytical Inc., USA). The powder and dry testing was also carried out on reference sample samples were measured under a 2θ scanning angle (MCC). Then DS value was calculated as follow from 10 to 80o at 0.03o/min increments. equations: Thermogravimetric analysis (TGA/DTG) was © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 74
25728288, 2023, S2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300070 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Extraction of microcrystalline cellulose from… performed on a SETARAM Labsys Evo 1600 vibrations of CH2 and CH groups, as well as angular (Setaram, Austria) in nitrogen atmosphere from room deformation vibrations of C-O-H. The absorption temperature to 800℃, heating rate 10oC/min. The peaks located at the wave number range of 1170-1060 morphology of the samples was observed by using a cm-1 are characteristic of cyclic monosaccarides and scanning electron microscope (SEM - Hitachi S 4800), correspond to valent vibrations of S-O and the C-C fitted with Oxford Instrument EDS probe. Curing ring structures. The presence of carboxylic acid behavior was investigated by a rheometer (MDR groups in maleated cellulose is clearly evident from a 2000, Alpha) at 160oC, ACS1 following ISO strong C=O stretching of carbonyl in the ester bonds 3417-2008. at 1721 cm-1, which indicates that the esterification reaction successfully occurred. There were no peaks 2.5. Mechanical properties for pure MA (1783 cm-1 attributed to symmetric stretching of C=O group, or 1856 cm-1 characteristic Tensile properties of NR and NR/cellulose composite for asymmetric stretching vibration of C=O group) were analyzed according to ASTM D412-92 using an found. It means that excess MA was completely AG-X Plus (Shimadzu - Japan) Universal Testing removed from MCC-g-MA. Machine, at speed of 500 mm/min, room temperature (30oC). 2.6. Swelling test The solvent resistance properties of the NR composites were evaluated following ASTM D471. The samples (20202 mm3) were cut and immersed in toluene at 30oC. They were removed every one hour interval and weighed until the solvent uptake was saturated. Solvent uptake (Wt%) = (W∞ – W0)*100%/W0 where W0 is the initial mass of the sample and W∞ is the equilibrium weight of sample. Figure 1: FTIR spectra of MCC (a) and MCC-g-MA (b) 2.7. Aging test Hot air aging process was carried out at 70°C for 72 h in a laboratory oven (EB 10Elastocon), following to ASTM D573. The mechanical properties of samples (according to D412-92) were evaluated before and after aging time for comparison. 3. RESULTS AND DISCUSSION 3.1. Extraction and maleic anhydride grafting of microcrystalline cellulose FTIR spectra of MCC and MCC-g-MA was shown in figure 1. Analysis of the characteristic oscillation regions of the samples showed all the characteristic regions of cellulose as published in the literature.[14] Figure 2: XRD patterns of MCC (MCC) and Actually, the figure shows the presence of a large MCC-g-MA (gMA) number of various types of hydrogen bonds, formed by –OH groups of macromolecules band in the field MCC has very high crystallinity, the crystalline of 3340 cm-1. The absorption band at 2900 cm-1 is region alternating with amorphous regions, each type attributed to the band of symmetric and asymmetric of cellulose has different origins and the percentage valent vibration of CH2 groups lies. The adsorption of crystallization is also different. XRD is one of the bands in 1660-1330 cm-1 are the deformation popular methods to investigate the parameters of © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 75
25728288, 2023, S2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300070 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Nguyen Ngoc An et al. crystallization region and crystallization density for The curing curve shows the minimum torque (ML) cellulose. Figure 2 presents the X-ray diffraction and maximum torque (MH), The scorch time (t’10), patterns of MCC and MCC-g-MA. They have a optimum curing time (t’90). These information’s was similar crystal structure. The main diffraction peaks summarized in table 2. The values of minimum torque are observed at 2θ = 14.8, 16.4, 22.7 and 34.9°, for (1 and scorch time are very close between each other. It 0 1), (1 0 -1), (0 0 2) and (0 4 0) diffraction planes, can be contributed to small volume of reinforcement. respectively. The grafting of MA onto the cellulose However, the maximum torque which is associated chain does not change the crystal region of cellulose, with the stiffness and crosslink density were higher in which could be explained, on the one hand, by the rubber compounds. The shorter optimum curing time small graft density, on the other hand, MA mainly was also observed in rubber compounds thank for reacts in the amorphous region. Thus, MA grafting presence of fillers. The similar results have been can cause a small change in the crystallinity of MCC. reported in other references.[1,16] As a result, the crystallinity index[15] calculated for MCC and MCC-g-MA were 90.2 and 92.9%, Table 2: Curing characteristics of of composites in accordingly. comparison with pure NR Scorch Torque Torque time t90 Samples Min Max ts10 (m:s) (dNm) (dNm) (m:s) NR 3.64 16.76 1:36 10:46 NR-M1 3.33 19.24 1:27 7:55 NR-Mg1 3.14 17.58 1:26 8:32 3.2.2. Mechanical properties Regarding tensile strength (table 3, figure 4), all composite samples showed a good improvement in Figure 3: TGA and DTG curves of MCC and tensile strength compared to pure NR, especially in MCC-g-MA samples containing a high percentage of fillers. NR- M7 and NR-Mg7 showed tensile strength values two Cellulose is not only biodegradable material, but times bigger than pure NR. It means that MCC can also a quite good thermal material. Figure 3 showed contribute significantly to the reinforcement of the thermal behavior of MCC and MCC-g-MA in a natural rubber. P. M. Visakh et al.[10] prepared temperature zone of 25-800oC. The results showed NR/cellulose nanowhiskers (CNWs) nanocomposites that two samples had a dehydration peak in the region that were extracted from bamboo pulp residue of a rounding 80oC. In this region, the MCC sample lost newspaper production. And they introduced a tensile 6.8% in weight, and the MCC-g-MA sample lost 5.6% strength of 17.3 MPa in a sample containing 10% in weight. It means that MCC-g-MA adsorbed less CNWs, while pure NR showed only at 9.2 MPa level. humidity than MCC. MA grafting makes MCC Additionally, tensile strength increases accordingly become more hydrophobic, which is an advantage in with increasing of CNWs. This tendency was also using modified MCC as a reinforcing phase for observed in our both series: with/without MCC-g- polymers materials. In higher temperature regions, MA. As mentioned above, MA was successfully the results showed no significant difference between coupled with MCC, and this unit can play a role as a the two samples. The decomposition temperature of compatible agent, double bonds of MA are expected both samples was about 365oC, and the to form chemical linking with the NR matrix to decomposition was almost complete when the ameliorate the interfacial interaction between them. temperature was raised to 500-600oC. The results of stress at 100 and 300% elongation And the degree of substitution (DS) of MCC-g- showed the same tendency as tensile strength (table MA was determined to be 0.12. 3). Stress at these elongations were enhanced when the percentage of fillers was increased. NR 3.2. Natural rubber microcellulose composites composites containing MCC-g-MA presented slightly higher stress at 100% elongation and 300% 3.2.1. Curing characteristics elongation than NR/MCC composite. Thus, MCC-g- © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 76
25728288, 2023, S2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300070 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Extraction of microcrystalline cellulose from… MA plays a certain role in the reinforcement of volume of fillers in the matrix, the more decreasing in NR/MCC composites. solvent uptake. However, solvent update reduction in NR/MCC-g-MA composites was around 1.5% bigger 20.0 than the ones in NR-MCC composites. This can be MCC contributed to the presence of MMC-g-MA which MCC-g-MA improved interaction between rubber chains and 15.0 MCC. Tensile strength (MPa) 10.0 5.0 0.0 0 1% 3% 5% 7% Percentage of filler (%) Figure 4: Tensile strength of composite NR/MCC and NR/MCC/MCC-g-MA in comparison with pure NR 3.2.3. Solvent resistance properties Figure 5: Solvent uptake of NR and NR composites Swelling test can be used to provide information about internal structure of NR composites. Swelling 3.2.4. Aging test studies of samples were performed in Figure 5 and Table 4. All samples absorbed toluene to make their Figures 6 and 7 showed tensile strength of NR and weight increasing. Solvent uptake increased quickly NR composites before and after aging test. There was in the 1-3 beginning hour of immersion, then slowly no significant change in tensile strength after 3 days down and got equilibrium weight after 8h. Regarding at 70oC.The similar trend was also observed in others NR and NR-MCC composite samples, the solvent publications.[19-21] The authors explained that MCC uptake of NR was 437.6%, which reduced was not undergo by such aging. After aging the significantly with volume percentage of MCC. The change in mechanical properties was mostly be reduction of toluene uptake can be explained by the contributed by NR itself and their vulcanizing interaction between matrix and reinforcements. The formulas. Sometime, aging test can improve Table 4: Equilibrium solvent uptake (wt%) of NR mechanical properties of NR composites which can and NR composites be explained by post cure effect.[21] Samples Equilibrium solvent uptake (wt%) NR 437.6 NR-M1 398.9 NR-M3 385.2 NR-M5 375.1 NR-M7 364.2 NR-Mg1 392.9 NR-Mg3 378.8 NR-Mg5 369.1 NR-Mg7 359.8 presence of MMC limited polymers chain’s mobility, and reduction of solvent uptake as a consequence.[17,18] The similar behavior in toluene swelling was Figure 6: Tensile strength of NR and NR/MCC observed in NR/MCC-g-MA composites, the more composites before and after aging © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 77
25728288, 2023, S2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300070 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Nguyen Ngoc An et al. 3.2.5. Morphology Surface investigation including elemental analysis of NR/MCC composite was performed by using SEM/EDS and the results were shown in Figure 8. MCC particles dispersed quite homogeneously in the sample at the micrometer level, there was no big aggregation of particles observed, even in matrix containing up to 7% in weight of NR (figure 8b). According to the images, dispersing diameter of filler was expected at a few micrometers, lower than 5 µm. It means that NR/MCC composite can be called a micro-composite. Figure 7: Tensile strength of NR and NR/MCC/MCC-g-MA composites before and after aging Table 3: Tensile properties of composites in comparison with pure NR Tensile Stress at Stress at Young’s Elongation at Samples strength Elongation Elongation Modulus break (%) (MPa) 100% (MPa) 300% (MPa) (MPa) NR 9.31±1.36 954.41±48.23 0.70±0.03 1.45±0.11 0.36±0.02 NR-M1 11.09±2.50 1263.10±46.65 0.74±0.06 1.45±0.16 0.41±0.02 NR-M3 13.33±1.60 1254.20±66.95 0.78±0.02 1.49±0.05 0.44±0.05 NR-M5 13.54±1.05 1271.19±32.46 0.82±0.06 1.57±0.14 0.48±0.01 NR-M7 17.29±3.52 1250.08±103.00 0.85±0.01 1.60±0.03 0.54±0.03 NR-Mg1 11.64±1.38 1088.41±88.20 0.75±0.06 1.46±0.14 0.43±0.02 NR-Mg3 13.51±1.93 1184.58±99.23 0.80±0.03 1.51±0.07 0.47±0.01 NR-Mg5 15.92±2.30 1332.13±61.16 0.85±0.04 1.56±0.10 0.51±0.06 NR-Mg7 18.96±0.95 1426.33±16.71 0.90±0.06 1.59±0.09 0.56±0.05 Figure 8: SEM images of NR-M3 (a), NR-M7(b), scanning zone EDS in NR-M7 (c), and EDS spectra of scanning zone (d) © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 78
25728288, 2023, S2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300070 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Extraction of microcrystalline cellulose from… However, SEM showed no evidence to compare the MCC was dispersed in NR matrix at a micrometer dispersion of particles in two series: NR/MCC micro- level. They can also slightly ameliorate the thermal composite and NR/MCC/MCC-g/MA micro- properties of NR. composite. This can be explained by a small percentage of fillers, actually 7% maximum is not a Acknowledgment. The authors gratefully big volume compared to other fillers for NR such as acknowledge the financial support of Vietnam carbon black, SiO2, etc. Elemental analysis (EDS) National University, Ho Chi Minh City, Vietnam for was also carried out for a zone of 60x60 µm (figure the research. 8c.d) on the surface observed. The results showed C and O as two main elements. It means that obersered REFERENCES area had cellulose. 1. H. Kazemi, F. Mighri, D. Rodrigue. A review of 3.2.6. Thermal properties rubber biocomposites reinforced with lignocellulosic fillers, J. Compos. Sci., 2022, 6, 183-215. P. Visakh et al.[10] presented also a thermal properties 2. H. Kazemi, F. Mighri, D. Rodrigue. Application of nanocelluloses in rubbers, J., Eds., Royal Society of improvement by cellulose nanowhiskers in their Chemistry: London, UK, 2021, pp. 38-65. composites, but we did observe clearly the same thing. 3. K. Roy, S. C. Debnath. A critical review on the Figure 9 showed the thermal behavior of NR in utilization of various reinforcement modifiers in filled comparison with NR/MCC at 7% (in weight of NR), rubber composites. J. Elastomers Plast., 2020, 52, the decomposition temperature of two samples was 167-193. found at 350oC, two graphs are almost overlapping 4. S. C. Peterson. Silica-milled paulownia biochar as which showed a very closed thermal properties of two partial replacement of carbon black filler in natural samples. However, the composite sample started to rubber, J. Compos. Sci., 2019, 3, 107. decompose later than the pure NR one. This can 5. S. C. Peterson. Coppiced biochars as partial attribute to the fillers. replacement of carbon black filler in polybutadiene/natural rubber composites, J. Compos. Sci., 2020, 4, 147. 6. N. A. Mohamad Aini, N. Othman, K. Sahakaro, N. Hayeemasae. Lignin as alternative reinforcing filler in the rubber industry: a review, Front. Mater., 2020, 6, 329. 7. C. S. Barrera, K. Cornish. Characterization of agricultural and food processing residues for potential rubber filler applications, J. Compos. Sci., 2019, 3, 102. 8. K. Roy, S. C. Debnath, A. Pongwisuthiruchte, P. Potiyaraj. Recent advances of natural fibers based green rubber composites: Properties, current status, and future perspectives, J. Appl. Polym., Sci. 2021, 138, 50866. 12. 9. M. J. John, R. D. Anandjiwala. Recent developments in chemical modification and characterization of . natural composites, Polym. Compos., 2008, 29, 187- 207. Figure 9: TGA curves of NR-M7 composite and 10. P. M. Visakh, S. Thomas, K. Oksman, A. P. Mathew. pure NR Crosslinked natural rubber nanocomposites reinforced with cellulose whiskers isolated from bamboo waste: 4. CONCLUSION Processing and mechanical/thermal properties, Composites: Part A, 2012, 43, 735-741. MCC was extracted from cotton fiber and applied to 11. P. T. L. Chi, N. N. An. A study on fabrication and NR as a reinforcing agent. The presence of MCC modification of microcrystalline cellulose (MCC) helped to improve tensile strength, elongation E100, prepared from cotton yarn, Science & Technology E300 of composite. Development Journal - Natural Sciences, 2022, 6(3), MCC was also grafted with MA and applied to 2287-2296. 12. H. F. Li et al. Study on the chemical modification of NR as a coupling agent for composites, tensile cellulose in ionic liquid with maleic anhydride, strength, elongation E100, E300 of composite Advanced Materials Research, 2012, 581-582, 287- containing MCC-g-MA is higher than composites 291. samples without a coupling agent. 13. S. Zeliko, J. Katarina, J. Slobodan, L. M. Dieter. © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 79
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