Preparation of Cu-modified bacterial cellulose aerogels derived from nata de coco towards the enhanced adsorption of non-polar organic solvents

doi:10.21203/rs.3.rs-2125333/v1

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Preparation of Cu-modified bacterial cellulose aerogels derived from nata de coco towards the enhanced adsorption of non-polar organic solvents

https://doi.org/10.21203/rs.3.rs-2125333/v1

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This study presented a simple and eco-friendly method to load copper nanoparticles on the surface of bacterial cellulose produced via the fermentation of coconut water by Acetobacter xylinum (Nata de coco). The Cu modification of BC surface was based on the reduction of copper (II) acetate by hydrazine under ambient conditions in a dispersion system of Nata de coco in water, which was followed by freeze-drying, affording lightweight Cu-containing cellulose aerogels. The structural features of the obtained aerogels were investigated by scanning electron microscopy with energy dispersive X-ray analysis (SEM/EDX), thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD), and nitrogen physisorption, indicating the high cellulose crystallinity, three-dimensional matrix and homogenous dispersion of Cu species on the cellulose bundles. The Cu-modified aerogel exhibited a significantly improved adsorption capacity of cyclohexane (66.4 g/g) as compared to that of pure cellulose (45 g/g). The excellent performances of 65.1-109.6 g/g were also observed for other non-polar solvents including n-hexane, toluene, ethyl acetate, dichloromethane, and chloroform depending their density.

bacterial cellulose

nata de coco

aerogels

non-polar organic solvents

Non-polar organic solvents play a key role in various chemical processes including organic reaction, purification, extraction, and manufacture of industrial materials [1–7]. However, the synthesis, transportation, and utilization of these compounds could lead to many dangerous chemical disasters, which have negatively affected the environment and human health. Therefore, it is important to dispose or recover these organic solvent after usage [8, 9]. And, one of the best approaches to treat them is employing adsorption methods because of its high efficiency, fast separation, simple manipulation, and reasonable cost [10, 11]. To ensure sustainable development for both humans and environment, it is critical to introduce green porous materials, which could apply to storage or remove non-polar chemicals from wastewater.

Recently, cellulose-based aerogels have attracted high interest from researchers due to their renewability, abundance and biodegradability [12]. Recently Quoc et al. have utilized the sugarcane bagasse for the preparation of cellulose-based aerogels coated with methyltrimethoxysilane (MTMS). A superhydrophobic surface after the surface functionalization with MTMS led to a good capacity for oil absorption (up to 25 g/g) [13]. Furthermore, instead of coating MTMS to enhance the hydrophobicity of cellulose, Li et al. developed superhydrophobic cellulose aerogels from natural sisal leaves by modification with Cu nanoparticles which was based on the simple reduction process from Cu²⁺ to Cu⁰ by hydrazine hydrate. The Cu-containing aerogels obtained via freeze-drying showed excellent adsorption performances for a large number of non-polar organic solvents (67.8 to 164.5 g/g) [14]. However, the application of plant cellulose usually requires many poisonous and complicated purification steps. Bacterial cellulose with high purity, three-dimensional structure and controllable production have recently emerged as a promising alternative for material science and technology [15]. In this study, bacterial cellulose derived from nata de coco which was obtained via the Acetobacter xylinum fermentation of coconut water was modified with Cu and subsequently freeze-drying, affording aerogel adsorbents towards efficiently trapping non-polar organic solvents.

All of the chemicals required for the experiments were purchased commercially from Sigma-Aldrich and Acros used directly without further purification.

2.1 Preparation of the materials

Preparation of nata de coco

Nata de coco was produced via the fermentation of coconut water, which was collected from the 8-month-old coconuts water in Ben Tre (Vietnam), by Acetobacter xylinum at ambient conditions. After 7 days, an approx. 2.0-cm layer of nata de coco formed on the surface of the liquid phase was collected and washed with sodium hydroxide solution (1 M) and water, respectively, until neutralization before being cut into 1.0-cm cubic pieces. The cellulose content in purified nata de coco was approx. 0.8 wt.%.

Preparation of cellulose aerogels modified with Cu nanoparticles (Cu NPs)

The Cu-containing aerogels were denoted as Cu-x-yz, in which x was the cellulose concentration (wt.%) in the freeze-dried mixture, y was the total cellulose mass (g) and z was the total Cu (II) acetate molar amount (mmol) (Figure 1 and 2). In a typical procedure to prepare Cu-0.24-13, the nata de coco cubic pieces (125 g) and water (125 g) were added to a 500 mL beaker and ground with distilled by hand blender Phillips HR1600 (550 W) in 6 min, affording a dispersion mixture of nata de coco in water. The resulting mixture (250 g, containing approx. 1.0 g of cellulose) was placed in a 1000 mL round–bottom flask before addition of copper (II) acetate (3.0 mmol) and subsequent stirring for 2 h. An 80% aqueous solution of N₂H₄.H₂O (50 equiv.) was dropwise added into the mixture for the reduction of Cu²⁺ to Cu⁰ for 14 hours at room temperature. After the reaction, nata de coco modified with Cu NPs was collected from the mixture by simple filtration and washed with distilled water until neutralization. The solid was re-dispersed in water with a cellulose concentration of 0.24 wt.% and frozen at -20 ^oC for 1 day before the freeze-drying process was performed for 72 h, finally affording the lightweight Cu-containing aerogel Cu-0.24-13.

2.2 Characterization of the materials

Powder X-ray diffraction (PXRD) patterns were recorded by a D8 Advance Diffractometer (Bruker AKS, Germany, Cu radiation). The data were collected in the range of 2θ from 10^oto 80^o with a step size of 0.01^o and a scan rate of 0.6^o/min.

Thermogravimetric analysis (TGA) was carried out by using the TA Instruments SDT Q600 Thermal Gravimetric Analyzer. To conduct the experiment, approx. 10 mg of the sample were heated from 40 – 900^oC at a rate of 10 ^oC/min in an air atmosphere.

The textural properties of the aerogels were investigated by nitrogen adsorption isotherm measurements at 77.4 K using an ASAP 2020 equipment. Prior to every adsorption experiment, samples were degassed at room temperature under vacuum for 6 h.

Scanning electron microscopy (SEM) images were obtained by a TM 4000 Hitachi microscope equipped with an energy-dispersive X-ray spectroscopy (EDX) detector from Bruker.

The average grain size analysis was performed on an LA-950V2 Laser Scattering Particle Size Distribution Analyzer Partica device.

2.3 Adsorption study

To investigate the trapping capacity for cyclohexane, the aerogel (m_aerogel, g) was immersed into a 100 mL glass bottle containing approx. 50 ml of cyclohexane (m_{bottle + cyclohexane} = m₁, g). After 5 min, the sample was gently lifted from the solvent until there was no more cyclohexane freely releasing. The total mass of the beaker containing cyclohexane was recorded as m₂ (g). The adsorption efficiency of Cu-modified material (Q) for cyclohexane was calculated by the formula Q = (m₁-m₂)/m_aerogel (g/g).

3.1 Characterization of Cu-modified aerogels derived from nata de coco

Cu NPs were loaded onto bacterial cellulose bundles in nata de coco by the aqueous reduction of Cu²⁺ to Cu⁰ in the presence of hydrazine hydrate as an efficient reduction reagent (Fig. 1a) [16, 17]. Upon the addition of hydrazine, the mixture colour steadily turned brownish-red, indicating the formation of the Cu(0) phase under ambient conditions (Fig. 1b and 1c) [14]. Instead of thermal drying under atmospheric pressure which resulted in a non-porous sheet-shaped product, freeze-drying was performed to yield the desired aerogel form. In the PXRD results shown in Fig. 3, two diffraction peaks at 2θ = 16.9° and 22.7° corresponding to the (110) and (020) lattice planes of crystalline cellulose were observed for both aerogel samples. The previous studies showed that a high-crystallinity phase of cellulose could be obtained in bacterial cellulose [14, 18]. The preservation of the cellulose-based features after loading Cu indicated that such a modification process had no effect on the cellulose structure. As expected, two additional sharp peaks were found at 2θ = 43.3°, and 50.5°, referred to the (111), and (200) planes of the pure metallic copper phase, respectively, obviously confirming the appearance of Cu in the aerogel. On the other hand, no Cu-based phases, namely, CuO, Cu(OH)₂ or Cu₂O were detected for Cu-0.24-13, demonstrating the high efficiency of this reduction pathway [19].

Table 1

Copper content in Cu-modified bacterial cellulose aerogels
Samples	Cu content (wt%)
Samples	Theory	Element analysis	TGA results
Cu-0.24-11	6.00	5.10	5.60
Cu-0.24-12	11.4	11.0	11.8
Cu-0.24-13	16.1	13.5	16.7
Cu-0.24-14	20.4	20.3	19.0

The TGA profile of the pure BC aerogel showed that the material was stable up to 270°C (Fig. 4). The thermal degradation was observed in the range from this temperature to approx. 400°C might involve many complicated reactions such as dehydration, depolymerization and oxidation, producing gaseous products, namely, CO₂, H₂O and other volatile compound [20]. Meanwhile the decomposition of the modified cellulose aerogel samples occurred earlier, at approx. 220°C, probably due to the presence of Cu species which could catalyze the thermal degradation of cellulose [21, 22]. Different from the almost complete decomposition of the unmodified sample, the residue mass for the Cu-containing samples occupied approx. 8–23 wt.%, depending on the initial Cu (II) acetate amount. Given CuO as the only remained phase of the thermal decomposition, the copper contents were determined to be 5.60, 11.8, 16.7 and 19.0 wt.% for Cu-0.24-11, Cu-0.24-12, Cu-0.24-13, and Cu-0.24-14, respectively. These values were close to the theoretical and ICP results, which were 5.10, 11.0, 13.5 and 20.3 wt.% for Cu-0.24-11, Cu-0.24-12, Cu-0.24-13, and Cu-0.24-14, respectively, indicating that the here-applied procedure allowed Cu to be efficiently loaded into the BC matrix (Table 1). The SEM images of the aerogels before and after the Cu modification presented the interconnected 3D framework constructed from bacterial cellulose fibers with the diameter of 40–60 nm (Fig. 5). Importantly, Cu species could be observed on the cellulose surface with a 13.4 wt.% content via the EDX analysis of Cu-0.24-13. It was therefore concluded that a good dispersion of Cu in the aerogel was obtained, thereby decreasing hydrophilicity of the aerogel towards the adsorption of non-polar liquids.

Non-ordered 3D arrangement of nanofibers could not only result in high toughness of nata de coco but also form a large number of pores with different diameters in the bacterial cellulose framework of nata de coco. This important textural property was maintained by freeze-drying, affording highly porous aerogels. N₂ sorption measurement of the pure BC aerogel exhibited the typical type IV isotherm with a hysteresis loop at the relative pressure range assigned to meso- and macropore, affording a BET surface area of 48 m²/g (Fig. 6) [23]. Though the aerogel form of BC after the Cu modification and subsequent freeze-drying was remained unchanged, independent on the Cu content, loading Cu species on the fibers and in the pores decreased the aerogel porosity, leading to a significant drop in the surface area to 11 m²/g (for Cu-0.24-13) [14]. Similarly, the total pore volume also remarkably decreased from 0.16 to 0.03 cm³/g. The effect of such textural changes on the adsorption efficiency of the Cu-modified BC aerogel would be elucidated in the next studies.

3.2 Adsorption studies

The appearance of copper nanoparticles played a key role in improving the cyclohexane capture of bacterial cellulose-based aerogels. Obviously, the cellulose fibers intrinsically owned a plenty of polar hydroxyl groups, which offered a weak interaction to the non-polar molecules and led to decrease in capturing these chemicals of materials derived from bacterial cellulose. Therefore, blocking or covering these functional groups by metal nanoparticles could help to adjust the hydrophobic property toward enhancing selective adsorption of hydrophobic organic solvents [14]. In this study, to take a deep understand regarding this effect on removal of cyclohexane, five materials with various amount of copper nanoparticles were prepared from the suspensions containing 0.24 wt% bacterial cellulose and different equivalents of Cu(CH₃COO)₂, including one equivalent (Cu-0.24-11), 2 equivalents (Cu-0.24-12), 3 equivalents (Cu-0.24-13), 4 wt% (Cu-0.24-14) and an unmodified Cu-aerogel sample (Cu-0.24-10) (Fig. 6). These aerogels respectively contained 5.10, 11.0, 13.5%, and 20.3% of copper nanoparticles, which was confirmed by element analysis. These samples were then applied in the cyclohexane adsorption study, which was conducted at room temperature in 5 minutes.

The adsorption capacity of the BC aerogels with varied Cu amounts for cyclohexane was investigated based. With high porosity, the Cu-free aerogel can adsorb 44.4 g/g of cyclohexane. When Cu species were present in the aerogel with a content of 5.10 wt.% (Cu-0.24-11), the cyclohexane-trapping capacity was significantly increased to 59.6 g/g (Fig. 7). As described above, loading Cu into the aerogel led to notable decreases in the surface area and total volume of the aerogel but a better performance was obtained. Such an adsorption enhancement could be attributed to the formation of the hydrophobic Cu NPs clusters in the aerogel, which partially covered the hydroxyl groups, thereby decreasing the hydrophilicity of the BC aerogel [14]. As a result, the non-polar organic solvents with a low surface tension easily access the aerogel framework, filling in the aerogel pores. Increasing the loaded Cu amount to 11.0 wt.% (Cu-0.24-12) yielded the cyclohexane adsorption capacity of 66.4 g/g. However, no further activity improvement was observed at the higher Cu contents, 13.5 wt% (Cu-0.24-13) and 20.3 wt.% (Cu-0.24-14) (Fig. 7). Obviously, the Cu excess was unnecessary to attract more cyclohexane molecules [14, 24].

In this work, freeze-drying was considered as the most essential step to maintain the 3D structure of the BC network in nata de coco, yielding the aerogel product. It was previously reported that the textural properties of aerogel was remarkably affected by the material concentration in the suspension system prepared prior to freeze-drying [23]. Indeed, the suspension mixture with a low concentration of Cu-modified cellulose (0.08%) led to the failure in the aerogel preparation. The dried solid showed poor mechanical features and almost no uptake of cyclohexane. At higher cellulose concentration (> 0.24%), the aerogels were obtained in a durable form. The experimental results showed that the adsorption capacity for cyclohexane gradually decreased from 66.4 to 40.3 g/g as the cellulose concentration increased from 0.24–0.72% (Fig. 8), which could be related to the density increase of synthesized materials, namely from 0.003 to 0.009 g/cm³. Obviously, with the same Cu amount, a low-density aerogel could produce a higher porosity, thereby trapping more cyclohexane in their structure.

Table 2

Median size of *nata de coco* based on LDS analysis at different grinding times.
Grinding time (minutes)	0	2	4	6	8	10
Median size (µm)	Not measured	679.75	565.03	330.51	284.47	237.27

Along with cellulose content, the size of nata de coco particles was found to have a great effect on the aerogel formation. Notably, freeze-drying Cu-modified cubic nata de coco pieces yielded a thin sheet, which showed a poor adsorption efficiency of 9.8 g/g due to its low porosity. It was observed that grinding could break nata de coco pieces into smaller fragments, leading to facile incorporation of cellulose networks. LDS analysis indeed revealed that the nata de coco size could be significantly decreased with the grinding time (Table 2). Therefore, the aerogel form could be obtained after freeze-drying such well-homogenized suspension mixture. As expected, the aerogel prepared via grinding in 2 min exhibited a much better cyclohexane trapping performance of 75 g/g as compared to the non-ground sample (Fig. 9). This adsorption capacity was remained unchanged as the grinding time increased to 4 min. However, the gradually declined efficiencies were observed for the aerogels based on Nata de coco ground with the further prolonged times, namely, 6–10 min. This could be rationalized by the fact that the 3D cellulose framework in nata de coco could be destroyed under exceeded grinding conditions, leading to the losses in the aerogel porosity as well as its adsorption capacity. It can be concluded that grinding nata de coco was indeed essential to produce the BC aerogels but the grinding time should be intensively considered to avoid unexpected structural collapses. Furthermore, the study on the adsorption time showed that the Cu-modified BC aerogel performed a high adsorption rate, reaching a cyclohexane-trapping capacity of 62.4 g/g within only 50 sec (Fig. 10). A saturation state at 75.1 g/g for the adsorption of cyclohexane was obtained after 5 min.

To demonstrate the great potential of the Cu-modified aerogel adsorbent derived from nata de coco, the study scope was expanded to other non-polar organic solvents, including n-hexane, toluene, ethyl acetate, dichloromethane, and chloroform. In general, the adsorption performance of the aerogel was directly proportional to the density of the organic solvents (Fig. 11). Among the tested solvents, the lowest trapping capacity of 65.1 g/g was observed for n-hexane with the density of 0.65 g/cm³ while 1 g of the Cu-containing aerogel can uptake 110 g of chloroform which possesses the highest density of 1.49 g/cm³. Compared to several previous studies on the utilization of cellulose-based materials for the adsorption of non-polar solvents, the Cu-modified BC aerogels prepared in this work exhibited the outstanding performances (Table 3). Most of these studies were focused on plant cellulose while the isolation and purification of plant cellulose fibers required many toxic chemicals and steps for the removal of lignin and other impurities which considerably affect the textural properties and adsorption activity. On the other hand, more efforts should be devoted to serapate, shorten, and tangle plant cellulose bundles from their rigid linear structure towards possible improvement in the porosity of prepared materials. Obviously, such disadvantages could be controlled via using high-purity bacterial cellulose with a natural 3D network of nanofibers, allowing the facile and efficient modification.

Table 3

Adsorption efficiency comparison of several cellulose-based aerogels
Solvent	Aerogel derived from cotton fiber	Aerogel derived from cellulose nanofibrils	Composite of keratin and cellulose	Cu-modifed aerogel derived from nata de coco
n-Hexane	19.8	25.0	7.1	65.14
Toluene	25.7	32.5	8.9	75.26
Chloroform	41.5	-	17.9	109.6
Reference	[25]	[26]	[27]	This work

In this work, a simple and environmentally benign approach was successfully introduced to prepare Cu-modified aerogels derived from bacterial cellulose in nata de coco. The resulting materials were fully characterized by various techniques to indicate the presence of well-dispersed Cu species on the bacterial cellulose surface, leading to the significant improvement in adsorption of cyclohexane. It was observed that the grinding time, cellulose concentration, and Cu content can have considerable effects on the free-drying-based preparation of the aerogel form as well as cyclohexane-trapping efficiency. The Cu-containing aerogel also exhibited impressive performance for other non-polar solvent, including n-hexane, toluene, ethyl acetate, dichloromethane, and chloroform. The formation of copper layers on the BC fibers could decrease the hydrophilicity of cellulose and affording a promising platform to design new materials, which could selectively and rapidly adsorb non-polar organic solvents.

Acknowledgements

This research is funded by Ho Chi Minh City University of Technology (HCMUT), VNU-HCM under grant number SVKSTN-2022-KTHH-13. We acknowledge the support of time and facilities from Ho Chi Minh City University of Technology (HCMUT), VNU-HCM for this study. We would like to thank Dr. Phuoc H. Ho for the characterization of aerogel materials.

Competing Interests

The authors have no relevant financial or non-financial interests to disclose.

Author Contributions

All authors contributed to the study conception and design. Material preparation, data collection and analysis were performed by Hanh H. M. Nguyen, Thanh T. T. Van, and Hanh N. Nguyen. The first draft of the manuscript was written by Hanh H. M. Nguyen, Thanh T. T. Van, Khoa D. Nguyen, and Ha V. Le and all authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.

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Preparation of Cu-modified bacterial cellulose aerogels derived from nata de coco towards the enhanced adsorption of non-polar organic solvents

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Abstract

Figures

1. Introduction

2. Materials And Methods

2.1 Preparation of the materials

2.2 Characterization of the materials

2.3 Adsorption study

3. Results And Discussion

3.1 Characterization of Cu-modified aerogels derived from nata de coco

4. Conclusion

Declarations

References

Supplementary Files

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