Modification of cellulose nanocrystals with 2-carboxyethyl acrylate in the presence of epoxy resin to enhance its adhesive property

doi:10.21203/rs.3.rs-810314/v1

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Modification of cellulose nanocrystals with 2-carboxyethyl acrylate in the presence of epoxy resin to enhance its adhesive property

https://doi.org/10.21203/rs.3.rs-810314/v1

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We synthesized the cellulose nanocrystals (CNCs) by using cotton as a raw material, then it was modified with 2-carboxyethyl acrylate to improve its adhesion and thermal properties. CNCs was chosen as a modifier to improve the interfacial adhesion between the reinforced nanocrystals and E-51 epoxy resin system. This gives a better modulus of elasticity, a lower coefficient of energy, and thermal expansion. Significant improvements in modulus properties, strength, transparency and thermal stability were observed with modified cellulose nanocrystals (MCNCs) compared with the standard sample. SEM, and transmission electron microscope (TEM), powder diffraction (XRD), (TGA and DTG) and Fourier transform infrared spectroscopy (FTIR) were used for the isolation of synthetic (native and modified) cellulose nanocrystals. In addition, the MCNCs adhesion properties with E-51 (Bisphenol A diglycidyl ether) epoxy resins were also investigated using the Zwick/Roell Z020 model.

Inorganic Chemistry

Biological Chemistry

Horticulture

Cellulose nanocrystals

Adhesion

Thermal

Modification

Reinforced

Cellulose nanocrystals (CNCs) are crystalline and rod shape depending on the source. It has also been used as reinforcing agent due to their excellent mechanical properties. [1–3] Its large surface area and intermolecular structure make them easily to interact. CNCs can form new resin bonds in compounds and improve mechanical strength of the final product. CNCs forms a cluster of networks with a relatively small amount and increase the flexibility modulus. [4, 5] substantially used as modifier to enhance the interfacial adhesion between nanocrystals matrix. [6–8] Cellulose has a natural nanostructure which can be detected by various methods and leads to the introduction of cellulose nanocrystals. The CNCs have width in range of 5 nm to 75 and length of more than 100 micrometers. [9, 10] Recently, uses of the CNCs as a modifier have been studied in a wide range of natural or synthetic polymers especially in epoxy emulsion. [11]

However, there are significant drawbacks in their use in such cases, particular due to their relatively low thermal stability. Therefore, it is very interesting to use their hydroxyl surface chemistry to give these nanoparticles a new functionality. There are many examples of CNCs editing routes. [12] Today, researchers in relation to current environmental issues to provide an affordable and scalable path for sustainable development have faced one of the most fundamental challenge. [13, 14] CNCs are a growing area for nanomaterials research candidates, because its attraction for reinforcing agent. Due to its reproducibility, high shear stress and elastic modulus up-to (100 GPa). [15, 16] It has high specific surface energy tend them to aggregate during the manufacturing process, forming larger particles. It is also found either in powder or in aqueous suspension after purification from amorphous cellulose or any other impurities and used in melt processing applications. [17, 18]

2-carboxyethyl acrylate is a new auspicious substitute monomer due to its molecular composition and replaces the mechanical properties of the less toxic, than the water-soluble monomers. Carboxyl group in the 2-carboxyethyl acrylate molecule has been expected to have a positive effect on the adhesive behavior of the CNCs suspension. [9, 19] 2-Carboxyethyl acrylate is more hydrophilic than inert monomer and provides chemical modification. It has better physical bonding to metal surface or other functionalities materials and may give better strength to the substrate. 2-carboxyethyl acrylate as an organic monomer which was used with CNCs to measure the mechanical strength. [20, 21]

Over the past decade, CNCs has been considered as a potentially natural nanomaterial and attracted researcher’s attention for its wide applications. The scattering and accumulation in polar solvents in a series of hashes attracted for optical and structural properties. These characteristics have a long-term effect on the overall performance and relationship. Here, we synthesized the cellulose nanocrystals (CNCs) by using cotton as a raw material, then it was modified with 2-carboxyethyl acrylate to improve its adhesion and thermal properties. CNCs were selected as modifier to improve the interfacial adhesion in E-51 epoxy resin. Therefore, in this preliminary work, CNCs play an important role for researcher, their properties and applications in different industrial sectors.

Guangzhou Liqi textile industry supplied the cotton. 2-carboxyethyl acrylate was purchased from J&K chemical. Analytical highly pure solvent was obtained from the Aladdin Shanghai industry. Tianjin Hengxing Chemical industry supplied the sulphuric acid: 98%. Bisphenol-A epoxy resin E-51 for adhesive property were supplied from Helin Resin Co., Ltd. Jiangsu province China. Potassium per-sulfate (KPs), and for curing Triethylenetetramine (TETA) (97.0%) were from Sigma-Aldrich.

2.1. CNCs preparation from cotton

To obtain cellulose nanocrystals (CNCs), firstly we removed the wax and pectin. 20 g of cotton is cut into small pieces and washed with hot water. The washed cotton is heated in a hot air oven at 40°C for 6–8 hrs. Then the cotton was mixed with 500 ml 20% NaOH solution at 45°C for 4–5 hours. Alkaline hydrolysis enhances the crystallization of cellulose nanocrystals. The alkali-treated cotton slurry is allowed to cool down at room temperature and the solution is transferred to 2.5 liters of distilled water until the pH is neutralized. The neutral suspension is filtered using a Buckner filter. Then heat the filtrate and stirred it in 500 ml 60% sulfuric acid for 12 hrs. at 35°C.

In this case, acid hydrolysis work to remove impurities such as hemicellulose and lignin. The cellulose suspension rapidly decomposes and the resulting particles form a white suspension transferred to 2 liters of water, to deactivate the white suspension. The suspension is suspended for 12 hours, allowing the suspension to be completely settled. The dilution solution was suspended. After decantation, the white slurry was again treated with distilled water to remove sodium and sulfate ions. The suspension is centrifuged at 8000 rpm three times for 10 mints. The nanocrystals were vigorously shaken in the 40°C range with 45–60 (w/v%) to remove completely H₂SO₄ solution. The final white product (CNCs powder) was dried in a vacuum oven at 90°C for 12 hrs., for further future properties and applications as shown in Figure-1.

2.2. Morphology of CNCs

A microscopic view of the native CNCs sample produced by the radio lens, seen through the microscopic surface morphology of the observation table as shown in Figure-2, many mesh formations were formed. The dimensions of the CNCs crystals were also observed. The results obtained show that the mean length is 103.47 nm and the mean width is 12.31 nm. 88.86% of the CNCs nanocrystals with a mean diameter which is 8.4 nm. The remaining crystals exhibited aggregation behavior due to the presence of a large amount of hydroxyl groups on the surface of the CNCs. [22, 23] The lower dose of CNCs showed a cluster like behavior, which may be higher and improving the interface, which is reflected in the rough surface layer. However, good dispersion is achieved even at low concentrations of CNCs with epoxy resins. The higher concentration of CNCs produces more surface inertia. The obtained CNCs crystals shape is rod like. CNCs TEM image revealed the presence of a compact, crystal-like, uniform nano-sized rod, which depend on their concentration in the epoxy system. [24]

2.3. 2-Carboxyethyl acrylate Modification with CNCs

Firstly, CNCs was dispersed in 40 ml of lab made distilled water at 60°C with stirring for 30 minutes at room temperature at N₂ environment. Then 66.6 mg potassium per-sulfate (KPS) was dissolved in 20 ml of distilled water, with the help of syringe were injected into the solution. After 30 minutes 2.1 ml of 2-carboxyethyl acrylate monomer was also injected and the reaction was allowed to stir at 60°C for 3 hours. The synthesis of CNCs-g-poly (2-carboxyethyl acrylate) was shown in Scheme-1.

Finally, the product was cooled down, then wash it with methanol 30 ml and water 70 ml mixture for 3 times with centrifugation 5000 rpm for 10 minutes, and then finally again wash with acetone to remove the ungrafted polymers, 3 times with same condition. Then the product was placed into the vacuum oven for 24 hours at 40°C to complete drying. After that the sample was put into the bottle and named it modified cellulose nanocrystals (MCNCs), saved in the desiccator for further investigating and characterizations.

2.4 Characterization

Modified cellulose nanocrystals (MCNCs) structure with 2-carboxyethyl acrylate was examined by FTIR (Nicolet. 5700). SEM, model SU-3500, analyzed under 20 kV were used for surface morphology. Transmission electron microscope TEM, Model Hitachi TEM system. TGA and DTG of the 2-carboxyethyl acrylate under constant N₂ flow were studied, while the crystallinity of CNCs and MCNCs was checked by XRD, KQ3200DB CNCs ultrasonic cleaner, ultrasound instrument Co., Ltd., was used for sonication. (Cence TG16-WS) Desktop high-speed centrifuge was used for washing modified CNCs. For adhesive properties (Zwick/Roel Z020) Germany model was used.

2.5. Adhesive strength test

E-51 epoxy resin was placed on the sample glass bottle, then the CNCs were added. The resultant mixture was sonicated at 45°C for more than 30 mins and then its suspension was prepared by mechanical mixing. The suspension was then circulated through the agitator until, all samples of CNCs are thoroughly dispersed in 1 g of E-51 epoxy resin at room temperature with magnetic bar for adhesive performance. After one hour stirring on hot plate at room temperature, 0.2 g of triethylenetetramine (TETA) was added and stirred slowly for the next 20–25 minutes until a completely homogeneous solution was obtained. The homogeneous solution was stored in a vacuum oven at 45°C for 10–15 min to remove bubbles from the solution. Then the entire mixture was poured onto steel plates as shown in Figure-3, using a 1.5 cm long and 2.3 cm wide glass rod. Three different samples with standard one was run for testing in a hot air oven at 150°C for 60 mins times. The samples were then cooled to room temperature, for 3–4 days prior to testing. To determine the mechanical properties, a Universal Material Testing Machine (model Zwick/Roel) Germany was used. The same procedure was adopted for modified cellulose nanocrystals (MCNCs).

3.1 CNCs-g-poly (2-carboxyethyl acrylate) FTIR analysis

The typical FTIR spectra of NCNCs and MCNCs is shown in Figure-4. A strong peak showed at 755 cm^− 1 was due to the C-H bending. [25, 26] The peak for C-O asymmetric in contrast to the spectrum of MCNCs was appeared at 1030 cm^− 1. A new vibration peak appeared at 1750 cm^− 1 was ascribed to the C = O group stretching vibration of the ester and carboxylic group present in MCNCs. [27, 28] Appearance of such peak in MCNCs giving confirmation the successful synthesis.

3.2 XRD analysis of CNCs and MCNCs

Crystalline structure of both nanocrystals was analyses by XRD as shown in Figure-5. The broad peaks revealed the appearance of crystal nature of CNCs. [31, 32] Two different peaks i.e., broad peak at 22° [33, 34] and the second peak of low intensity at 34°, remained in MCNCs. However, MCNCs showed low crystal latency than native CNCs. In contrast, the additional native cellulose nanocrystals peak at 15° is no longer available in MCNCs. Crystallinity has almost removed in MCNCs such loss of peak at 15° decrease in intensity of peak at 22° and almost completely disappearance of peak at 34°. [35, 36]

3.3. Adhesive properties of MCNCs

We have also studied the adhesive properties of MCNCs with epoxy system, as shown in Figure-6. The average shear strength and shear modulus is mention below, using E-51 epoxy resin with different content. As mentioned above (TETA) used as a curing agent. E-51 epoxy system containing MCNCs in an amount of 1, 3, and 5 wt% to evaluate the effect of adhesive properties.

The shear strength shows higher enhancement at 5 wt% of MCNCs. It is the possible cause of crystals agglomeration in the epoxy resin medium which make them harder. [37, 38] The maximum value was observed at 15.1 (MPa) for nanocomposites reinforced with 5 wt% MCNCs compared with the pure epoxy resin [39].

In compared with the standard sample, all the MCNCs samples had a higher shear modulus. The maximum value was observed 2460 (MPa) for 1 wt% modified nanocrystal in compete with the standard value which is 1990 (MPa). We believe that the result of MCNCs with E-51 epoxy resin, -OH bond is responsible for binding themselves. Creating a high strength linkage and increasing the adhesive additives properties. MCNCs shear modulus loading (5-wt%) agglomeration and aggression occurs between particles in epoxy system, which produce weakness. [40, 41]

In this study, we synthesized CNCs and then observed their different properties and applications. Cellulose nanocrystals matrix successfully modified by 2-carboxyethyl acrylate using modification approach. CNCs matrix modification has been verified through different spectroscopic techniques. MCNCs study as reinforce material for different polymers have been found processing good adhesive performance, achieved high shear strength 15.1 (MPa) at 5 wt% and modulus 2460 (MPa) at 1 wt%. 2-carboxyethyl acrylate introduction to CNCs have significant effects on physicochemical properties of CNCs. MCNCs of adhesive properties are improved due to the dispersion and better interaction between grafted CNCs and the E-51 epoxy system. CNCs consist of linear polymers without water units, connected to one of four carbon atoms via the β-glycosides bond. Therefore, in this preliminary work, CNCs play an important role in different industrial applications.

Statement

We have no conflict of interest.

Acknowledgments

This research was funded by the State Key Laboratory of Chemical Engineering, Zhejiang University 310027 Hangzhou, China

Sources of financial funding and support

This research work is not funded by any agency.

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Scheme1.png
Synthesis of CNCs-g-poly (2-carboxyethyl acrylate)

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Modification of cellulose nanocrystals with 2-carboxyethyl acrylate in the presence of epoxy resin to enhance its adhesive property

Status:

Version 1

Abstract

Figures

1. Introduction

2. Method And Chemical Reagents

2.1. CNCs preparation from cotton

2.2. Morphology of CNCs

2.3. 2-Carboxyethyl acrylate Modification with CNCs

2.4 Characterization

2.5. Adhesive strength test

3 Results And Discussion

3.1 CNCs-g-poly (2-carboxyethyl acrylate) FTIR analysis

3.2 XRD analysis of CNCs and MCNCs

3.3. Adhesive properties of MCNCs

4 Conclusion

Declarations

References

Supplementary Files

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