Sustainable extraction and physicochemical characterization of nano-lignin derived from jute-based agro-industrial biomass

Abstract

The aim of this research was to extract lignin from jute-based agro-industrial biomass and synthesize nano-lignin particles using a sustainable solvent-anti-solvent precipitation process, followed by the physicochemical characterization of the synthesized particles. Different characterization techniques such as FTIR, SEM, EDX, DLS, XRD, Zeta Potential, TGA and DSC were carried out to evaluate the structural and physicochemical characteristics of the synthesized nano-lignin particles. FTIR analysis showed the presence of important lignin functional groups such as hydroxyl (3316 cm^-1), carbonyl (1650 cm^-1), aromatic groups (1419 cm^-1) and C-O groups and similar characteristic peaks were observed after nano-lignin synthesis. SEM analysis revealed irregular, porous, fragmented and heterogeneous surface morphology of the synthesized particles, which is consistent with the commonly reported characteristics of nano-lignin particles. DLS analysis showed an average particle size of around 117 nm, with uniform particle size distribution. The zeta potential value was found around -35 mV (millivolt), suggesting comparatively good colloidal stability and dispersion behavior of the synthesized nano-lignin particles. XRD analysis indicated, predominantly amorphous structural characteristics, which are consistent with the traditionally reported amorphous characteristics of lignin-based nanoparticles. EDX analysis showed that carbon and oxygen were dominant detected elements in the synthesized samples. TGA and DSC analyses suggested that the synthesized nano-lignin particles exhibited multi-stage thermal degradation behavior. Overall, this research reported a sustainable approach for lignin extraction and nano-lignin synthesis from jute-based agro-industrial biomass. Further studies may be carried out to investigate the synthesized nano-lignin particles through more detailed and advanced characterization techniques.

Keywords

jute stick lignin nano-lignin organosolv method characterization sustainable materials

Introduction

Each year, Bangladesh produces a large amount of jute stick biomass, and after jute fiber extraction, most of it is considered an agro-industrial residue. In spite of containing a considerable amount of lignin, jute stick biomass is often underutilized and is mainly used as low-value fuel material resulting in inefficient biomass valorization. Jute sticks are easily available in Bangladesh and contain a significant amount of lignin that is why it is considered a potential source of lignin production.

Lignin is a natural aromatic biopolymer that has gained increasing attention for sustainable bio-based material development. Lignin in nano form exhibits improved surface area, colloidal behavior, and physicochemical properties.¹ This research is important in the field of sustainable lignin extraction from jute-based agro-industrial biomass and its subsequent advanced physicochemical characterization.

Jute biomass is an agro-industrial byproduct that is associated with the textile sector. Raw jute sticks are abundantly available in Bangladesh. For this research, jute sticks were collected from the Nuthurchar area of Gopalpur, Tangail region and then they were made into powder form following some laboratory processes. After that by the ethanol organosolv method, lignin was extracted from jute stick powder through some laboratory processes. Once the lignin was extracted, it was converted into nano-lignin form and then subsequent advanced characterization techniques were performed.²

Different scholars worked related to this experiment at different times where literature review exposed different results, some of which were similar and some were widely dissimilar. Due to the ranges of variables involved like pH, time, temperature and chemical concentrations, the result of lignin extraction were drastically changed.³

To reduce reliance on fossil-based resources, ligno-cellulosic biomass has gained substantial attention as a sustainable resource to produce materials and chemicals. Amongst the main constituents of ligno-cellulosic biomass, lignin is the most important natural polymer that retains a complex aromatic structure. Because of these exclusive features, lignin has been developed as a promising material for uses in polymer composites.⁴

Jute is one of the most important natural crops in Bangladesh that generates a large quantity of jute stick as a cultivated by-product after fiber extraction. Usually, jute sticks contain a significant amount of lignin around 20–25%. Several methods have been described for lignin extraction from ligno-cellulosic biomass, comprising acid, alkaline and organosolv methods. Among these, the ethanol organosolv method has attracted attention because of its comparatively low ecological influence and its capability to generate high-purity lignin.⁵

Presently, the progression of nanotechnology has facilitated the transformation of bulk lignin into nano-lignin, which shows improved surface area, enhanced reactivity, and better diffusion characteristics. In most researches, lignin has been extracted from common natural resources like wood, bamboo and agricultural residues, whereas study on lignin extraction from jute stick is still limited.⁶

Besides, precise synthesis of nano-lignin from jute stick with even particle size and enhanced stability has not been widely explored. Also, the physicochemical characterization of jute-derived nano-lignin particles is still limited. So, there is a need for methodical examination into ecological extraction techniques and effective nano-lignin synthesis from jute stick biomass.⁷

Jute sticks are generally composed of cellulose (40-45%), hemicellulose (20-25%), lignin (20-25%) and minor quantities of extractives (3-5%) and ash (1-2%). The composition may differ depending on the type of jute cultivation conditions and harvesting procedures. However, jute sticks normally contain a substantial amount of lignin compared to other agricultural residues, making them an appropriate raw material for lignin extraction.⁸

Researchers studied and characterized lignin extraction from jute fibers and sticks using FTIR and NMR, but they did not use advanced characterization techniques such as SEM, EDX, DLS, Zeta Potential, XRD and TGA. Researchers studied the structural characterization of lignin extracted from jute biomass; but they did not investigate nano-lignin synthesis process.⁹ Earlier studies showed that researchers investigated the effect of chemical processing on the structural and physicochemical characteristics of lingo-cellulosic materials and biomass-based systems.¹⁰

In earlier studies, researchers investigated the cellulose-based materials and analyzed their structural and physicochemical characteristics under different processing conditions.⁸ In the past studies, researchers investigated the structural and thermal behavior of cellulose-based materials under different processing conditions.¹¹

In related studies, researchers investigated the structural and physicochemical characteristics of cellulose-based materials under different processing conditions and exposed their material characteristics using different experimental techniques.¹² In the published studies, researchers investigated the influence of different processing conditions on the structural and physicochemical characteristics of cellulose-based materials using microscopic analysis techniques.¹³

Recent studies have demonstrated that chemical treatment of lingo-cellulosic biomass can effectively modify its physicochemical characteristics and improve its performance in material-based systems.¹⁴

In earlier studies, natural bio-based compounds have been investigated for sustainable coloration of cellulose-based materials.¹⁵ Several researchers investigated sustainable cellulose-based materials and analyzed their physicochemical characteristics using advanced techniques such as FTIR spectroscopy.¹⁶

According to the literature, researchers investigated sustainable biomass-derived materials and their structural and physicochemical characteristics.¹⁷ A group of researchers investigated sustainable biomass-derived materials and analyzed their physicochemical characteristics using advanced analytical techniques such as FTIR spectroscopy.¹⁸

In recent years, researchers have studied biomass-derived composite materials using sustainable natural fillers to improve the structural and physicochemical characteristics of advanced materials.¹⁹ A group of researchers indicated that biomass-based fillers significantly affect the morphology and thermal behavior of composite systems, highlighting the importance of comprehensive characterization techniques including FTIR, SEM, and thermal analysis in sustainable material research.²⁰

From the reviewed studies, it was observed that the key gaps were found in nano-lignin synthesis and its advanced characterization techniques. Although ethanol organosolv extraction and solvent–anti-solvent precipitation are established methods, studies on the extraction, synthesis, and advanced physicochemical characterization of nano-lignin derived from jute-based agro-industrial biomass remain limited. Therefore, the present study focuses only on the sustainable production of nano-lignin from under-utilized jute biomass and its detailed characterization using multiple advanced analytical techniques such as FTIR, SEM, EDX, DLS, zeta potential, XRD, DSC, and TGA to evaluate its physicochemical and structural properties. However, application performances were not evaluated in the present study.

Materials and method

Raw materials used

For this research, jute sticks were collected in the DUET Laboratory from the Nuthurchar area of Gopalpur, Tangail district in Bangladesh. The collected jute sticks were washed using tap water to remove dust particles. Afterward, the jute sticks were dried in sunlight for a day on the rooftop of DUET textile engineering laboratory building. Figure 1 shows the Preparation of Jute Powder from Raw Jute Stick using a laboratory grinder. Figure 1(a) shows raw jute stick, Figure 1(b) shows the cleaning process of raw jute stick using normal tab water, Figure 1(c) shows the grinded jute stick and Figure 1(d) shows the final powder of raw jute stick.

Figure 1.

Preparation of Jute Powder from Raw Jute Stick using laboratory grinder.

After drying, the jute sticks were cut into small pieces of approximately 1cm. Using a grinding machine in the laboratory, the jute pieces were grinded into powder form. The prepared jute stick powder was then stored in an airtight container for further characterization techniques.

Chemicals used

96% analytical grade ethanol (Merck Germany) and glacial acetic acid (99-100%) (Merck Germany) were used in this investigation to extract lignin from raw jute powder. Distilled water was also used for solution preparation. A Solvent-anti-solvent precipitation process was followed to obtain lignin and nano-lignin powder from jute stick. All the chemicals used in this research were of analytical grade and were used without further purification.²¹

Extraction method of lignin

At first, cleaned, and dried jute sticks were collected and cut into small pieces (jute sticks were cut into 1 cm of small pieces). Using a grinder machine in the laboratory, the jute pieces were crushed into powder form. For lignin extraction, 20 g of dried jute stick powder was collected in a beaker. Then slowly 400 ml of ethanol-water solution (60:40) was mixed with the powder. Therefore, the solid to liquid ratio became 20:400 or 1:20.

Figure 2 shows the extraction process of lignin from jute sticks. Figure 2(a) shows the extraction process of lignin in magnetic stirrer. Figure 2(b) shows the Dark brown colored solution containing lignin after filtration from magnetic stirring. Figure 2(c) shows the Dark brown colored solution containing lignin after filtration from magnetic stirring. Figure 2(d) and (e) shows the extracted lignin powder from Jute sticks.²²

Figure 2.

Extraction process of lignin from jute stick.

The solid to liquid ratio was maintained 1:20. The extraction conditions were selected following previously reported lignin extraction methods for lingo-cellulosic biomass. At this stage, the pH was initially measured at approximately 8-9. 1-1.5ml of acetic acid was then added into the solution to keep the bath pH 4-5. Using a magnetic stirring machine, the mixture was then heated at 80–90 °C for 8-10 hours to get a dark brown colored solution. The pH and extraction temperature were adjusted based on initial experimental observations to obtain a stable lignin-rich solution. This dark brown solution contained dissolved lignin materials.²³

Based on the solvent solute ratio calculation, 400ml of solution was prepared by mixing ethanol and water in a 60:40 ratio. Accordingly, the ethanol volume was 240ml, while the water volume was 160ml.

After that the mixture was filtered using filter paper to separate cellulose/hemi cellulose rich solid residue, and the lignin solution was obtained as the filtrate. Distilled water was then added to the lignin solution at a ratio of 1:3 to precipitate the lignin particles. A centrifugation process was subsequently carried out to precipitate the lignin particles in the test tubes. The lignin particles were collected by filtration using filter paper with a pore size of 2.25µm. The lignin particles were dried in an oven at 50°C temperature over night to obtain dried lignin powder.²⁴

Nano-lignin synthesis

At first, 1 g of lignin powder was mixed with 100ml of ethanol under continuous stirring to obtain a homogeneous solution. This homogeneous solution was then added dropwise into 800 ml of distilled water under constant stirring into a beaker.

This change in solvent polarity led to the formation of nano-lignin particles into the beaker. The mixture was then stirred for around 30 minutes to ensure uniform particle formation.²⁵ Centrifugation was then carried out for 10 minutes at 3000rpm to obtain precipitated nano-lignin. Figure 3(a) shows the nano-lignin synthesis process and Figure 3(b) shows the extracted jute nano-lignin powder.

Figure 3.

Nano-lignin synthesis process.

This nano-lignin was then filtered using a membrane filter with a pore size of 0.45µm and dried in an oven at 50°C temperature over night to obtain dried nano-lignin powder. During this process, approximately 10-15% material loss was observed since 0.8-0.9 g of nano-lignin was collected from 1g of lignin powder.²⁶ In this process, lignin was converted into nano-lignin using a solvent anti-solvent precipitation process. Nano-lignin was synthesized using a solvent exchange mechanism. Rapid change in solvent polarity leads to the precipitation of lignin particles into lignin nano particles.²⁷

In this study, approximately 0.8g to 0.9g of nano-lignin powder was obtained experimentally from 1g of lignin powder.

Since, after synthesis, sometimes 0.8g of nano-lignin was obtained and sometimes 0.9g of nano-lignin was obtained from 1g of lignin. So, the minimum and maximum yield% were calculated.

So, the maximum & minimum yield% for the nano-lignin synthesis was 80% to 90% with an average yield% of 85%.

In the extraction process, 1g of lignin was first dissolved in 100ml of ethanol. After that 800ml of distilled water was added dropwise to the solution to introduce precipitation. So, the solvent to anti solvent ratio was 1:8 after basic calculation.

Characterization techniques

After lignin extraction and nano-lignin synthesis process from jute sticks nano-lignin, different characterization techniques were carried out like FTIR, SEM, EDX, TGA, DSC, DLS, XRD and zeta potential. These characterization techniques were used to evaluate the structural and physicochemical characteristics of the synthesized lignin nano-particles. These characterization techniques were used to evaluate the particle size, surface structure, chemical structure and their stability.

FTIR analysis

FTIR (Fourier Transform Infrared) analysis was carried out to identify the functional groups in lignin and nano-lignin. In this analysis, the spectrum wavenumber range was 4000–400 cm^-1. The obtained peak values indicated the presence of hydroxyl, carbonyl and aromatic groups in lignin and nano-lignin. FTIR analysis also helped to examine the retention of the major functional groups after the nano-lignin synthesis process.

SEM analysis

SEM analysis was used to observe the surface morphology and structural characteristics of the lignin nano particles. SEM provided the high-resolution images of the synthesized nano particles and their surface morphology. Nano-lignin showed circular or irregular shaped nano-particles. Besides, SEM images also helped to identify whether there was aggregation and clustering of particles.

DLS analysis

The full form of DLS is Dynamic Light Scattering that was used to examine the particle size and distribution of nano-lignin. It showed the hydrodynamic diameter of nano particles, which provided information regarding the behavior of nano particles in liquid state. By this process, the Poly dispersity Index (PDI) can be measured, which indicated the uniformity of nano particles. Lower PDI values indicate a more uniform particle size distribution and vice versa.

XRD analysis

The full form of XRD is X-ray Diffraction analysis. XRD analysis was carried out to determine the crystallinity and structural characteristics of nano-lignin particles. Pure lignin is an amorphous substance and it showed a broad peak in graph. The analysis helped to evaluate whether the original structure of the lignin had changed during nano synthesis process or not. It is useful for suggesting the structural stability of nano-lignin.

Zeta potential analysis

Zeta potential analysis was used to evaluate the surface charge of nano-lignin particles and their colloidal stability in suspension. These values showed the electrostatic repulsion between the particles, which prevented their aggregation. High positive or negative values of zeta potential indicate better dispersion stability and vice versa. It also helped in understanding the suspension character of nano-lignin particles.

TGA analysis

TGA stands for Thermo-Gravimetric Analysis. TGA analysis helped to determine the thermal stability and degradation behavior of nano-lignin. In this process, the change in sample weight was observed with the increase of temperature. Generally, at first, due to the increase in temperature in TGA analysis, moisture loss occurs and then happened the degradation of lignin structure.

Results and discussion

This section discusses the results of the study. Different types of characterization were performed like TGA, SEM, Zeta Potential, XRD, DLS, FTIR and their findings will be discussed. These results support the structural and physicochemical characterization of synthesized nano-lignin particles. These results are obtained after the extraction and synthesis process of nano-lignin.

Results of FTIR

FTIR analysis showed the functional groups present in lignin and nano-lignin particles. Figure 4 shows the FTIR spectrum of nano-lignin from jute stick. It has two axes, one axis is Transmittance (%) and another axis is wavenumber (cm^-1). Wavenumber indicates the functional group and transmittance% indicates the absorbance. The amount of light is passing through the sample is expressed via T%. The higher values of transmittance T% expressed low absorption and vice versa. Also, the higher absorbance values indicate stronger peaks and vice versa.²⁸

Figure 4.

Ftir observation of nano-lignin.

The FTIR values were observed in the range of 400 to 4000 cm^-1. In this FTIR figure, absorption peaks indicate the presence of the functional groups. The peak value at 3316.96 cm^-1 indicates the presence of hydroxyl group. The peak value at 2333.45 cm^-1 may be associated with atmospheric CO2 absorption in the nano-lignin particles. The peak value of 1650.77 cm^-1 indicates the stretching vibration of carbonyl (C=O) group. The peak value of 1419.35 cm^-1 suggests the vibration of aromatic ring, which is the main structural part of nano-lignin. The peak value of 1056.8 cm^-1 indicates C–O stretching vibration that indicates the presence of alcohol, ether, and phenolic groups in nano-lignin. The peak value of 539.97 cm^-1 indicates aromatic structure and it’s bending vibration.²⁹ The observed FTIR peaks were consistent with the characteristic functional groups widely reported for lignin in related studies.

It can be observed from this FTIR spectrum that the major functional groups of lignin, such as hydroxyl, carbonyl, and aromatic groups were still present after the synthesis of nano-lignin. The overall interpretation suggests that the major characteristic functional groups of lignin were retained in the synthesized nano-lignin particles.³⁰

Table 1 shows the presence of the important functional groups in lignin structure along with their peak values. The values presented in Table 1 suggest that all the important functional groups of lignin were present in the extracted lignin nano particles.

Table 1.

Presence of the functional groups in lignin structure in FTIR Observations.

Functional group observations	Attained values (cm^-1) in FTIR	Reported values (cm^-1) ranges from previous studies	Statements
Hydroxyl (–OH) stretching	3316.96	3200–3600	OH group is present in the lignin structure
Carbonyl (C=O) stretching	1650.77	1600–1700	Carbonyl group is present in the lignin structure
Vibration of the Aromatic ring	1419.35	1400–1600	indicates aromatic structural characteristics
C–O stretching	1056.8	1000–1100	Suggests the presence of Alcohol, ether, and phenolic group in lignin
Aromatic bending	539.97	500–700	Suggests aromatic structural deformation vibration of lignin

Results of SEM

SEM (Scanning Electron Microscopy) was used to investigate the surface morphology and structural characteristics of the synthesized nano-lignin particles. Different structural images of jute nano-lignin like surface morphology and aggregated particle structures were displayed clearly. Each image was taken at different magnifications levels to understand the structural characteristics properly.³¹

The Figure 5(a) was captured at the scale of 10µm (micrometers) scale bar, where the angular and broken structures of nano-lignin were clearly visible. In the figure, several small structures were noticed those indicated the complexity and complex morphology of jute nano-lignin particles. Irregular and fragmented particle clusters were also observed, which indicates the heterogeneous morphology of the lignin nano particles.

Figure 5.

SEM images of nano-lignin derived from jute biomass at different magnification.

Figure 5(b) was recorded at higher magnification with a 1um scale bar, the structures were seen finer and relatively rounded structures and some small holes were visible. Some particle agglomeration was observed in the structures, which may be due to lignin nanoparticles had high surface energy and intermolecular interactions during drying and sample preparation.

Figure 5(c) revealed the clustered, broken, and irregular surface structures of the synthesized nano-lignin particles. In the molecular structures on nano-lignin, some separations or reduction parts are there, which may contribute to higher surface irregularity. The observed aggregation behavior of the lignin nano particles may be attributed to hydrogen bonding interactions.

The Figure 5(d) was captured at the scale of 1 µm (micrometers) scale bar, where the structure was seen thicker and smoother. These images clearly exposed the structural shapes of the lignin nano particles. These images showed the formation of nano-structured lignin particles with heterogeneous surface morphology.

The Figure 5 (a)-(d)nano-lignin showed, the fine and nano-structured morphology and porosity of jute nano-lignin, which revealed the porous and heterogeneous morphology of nano-lignin particles.

The micrometer-scale bars in the SEM images represented the observation scales of the micrographs and did not indicate the actual primary particle size of the nano-lignin particles. The nanoscale particle size was supported by DLS analysis that showed an average particle diameter of approximately 117 nm.³²

Results of EDX

Energy Dispersive X-ray (EDX) analysis was carried out to identify the elemental composition of the synthesized jute nano-lignin samples.

In Figure 6, EDX Spectroscopy of Jute Nano-lignin was presented. The X-axis showed the keV (kilo electron volt) values that indicated X-ray energy level, while the Y-axis indicated the counts of X Rays detection. The higher the peak is the higher the presence of the element is and vice versa. In Figure 6 and in Table 2, the weight% of Carbon (58.55%) and Oxygen (41.45%) were seen those falls in between the frequently reported values ranges for extracted lignin particles. From the detection, it was seen that carbon and oxygen were the dominant detected elements. The calculated carbon/oxygen ratio was 1.41, which supported the aromatic and carbon/oxygen containing functional nature of lignin.³³

Figure 6.

EDX Spectroscopy of treated Jute Nano-lignin.

Table 2.

Elemental Composition% for treated Jute Nano-lignin.

S.N	Element	Energy (keV)	Atomic (%)	Sigma	Weight (%)	Normally reported (%)	Remarks
1	C (K)	0.277	65.29	0.23	58.55	50-65	Within the expected range
2	O (K)	0.525	34.71	0.49	41.45	30-45	Within the expected range
Total			100		100

Lignin is a complex aromatic biopolymer that is mainly composed of phenylpropane units and typically contains high level of carbon and oxygen. The obtained result was consistent with the reported elemental characteristics of lignin. The relatively high Carbon content may be associated with the aromatic ring structure of lignin, while the Oxygen content may indicate the presence of Oxygen containing functional groups such as hydroxyl (–OH), methoxy (–OCH₃) and carbonyl (C=O) groups.³⁴

Figure 6 indicated that carbon and oxygen were the dominating constituents present in the synthesized nano-lignin sample.

The presence of dominant carbon and oxygen peaks indicated that the sample was organic in nature and possessed elemental characteristics often associated with lignin-based materials. Hence, the results demonstrated from the EDX analysis that the obtained elemental composition was consistent with the broadly reported characteristics of lignin-based materials.³⁵

Results of DLS

Dynamic Light Scattering (DLS) was used to determine the hydrodynamic particle size and particle size distribution of the synthesized nano-lignin. Figure 7 shows the Dynamic Light Scattering graph, where the X-axis represents the hydrodynamic diameter and the Y-axis represents the intensity% of the nano-lignin particles, indicating their relative particle size distribution. This report was prepared using Malvern Panalytical Ltd. (UK) at 25°C temperature. The particle size and distribution of the prepared jute nano-lignin were measured at this temperature using water as dispersant.³⁶

Figure 7.

Dls graph of derived nano-lignin from jute stick.

From Table 3, the results indicate that the Z-Average hydrodynamic diameter was 117.25 nm, which falls within the largely reported size range of the nano-lignin particles. These results suggest the effectiveness of the solvent anti-solvent precipitation method for producing nano sized lignin particles from jute biomass. The regularly reported value ranges for the hydrodynamic diameter is generally in between 50 to 300 nm.

Table 3.

DLS Values of the tested Jute Derived Nano-lignin.

S.N	Description	Obtained values	Reported value ranges from earlier studies	Remarks
1	Mean Count Rate (kcps)	282.3	200–500 kcps
2	Run Retention (%)	93.33	greater than 90%
3	Fit Error	0.01254	less than 0.02
4	Intercept	1.016	in between 0.9 to 1.05
5	Poly-dispersity Index (PI)	0.1015	less than 0.2
6	Z-Average (nm)	117.25	values in between 50 to 300 nm	values in between 50 to 300 nm is consistent with previously reported values for nano-lignin particles
7	Peak 1 Area by Intensity ordered by size (%)	10.1	Less than 20%
8	Peak 1 Width by Intensity ordered by size (nm)	4.09	lower is better
9	Peak 2 Area by Intensity ordered by size (%)	90.01	more than 70%
10	Peak 2 Mean by Intensity ordered by size (nm)	120	values in between 80–200 nm

The PDI value of the sample nanoparticles was 0.1015 that indicates the narrow and uniform particle size distribution. This is the characteristic of a comparatively well dispersed nano particle system. The standard PDI value generally ranges from 0.1 to 0.3.³⁷

In the analysis of Intensity based particle size distribution, a major peak was observed at approximately 120 nm, representing about 90% of the total particle distribution. Besides, a small peak around 45.02nm represented nearly 10% of the particle size distribution. This observation indicates that the sample mainly contained a dominant particle size distribution.³⁸

The fit error value of the DLS analysis was 0.01254 (lower) and the intercept value was 1.016 (near to 1), which indicated the satisfactory signal quality and measurement reliability. The conventionally reported fit error values generally lie in between 0.01 to 0.1, while the intercept value is generally expected to remain close to 1.0.

The mean count rate was 282.3 kcps and the run retention value was 93.33% that indicated the experiment was conducted under a stable and reliable condition. The predominantly reported mean count rate generally ranges from 100 to 500 kcps, while run retention values above 90% are considered acceptable. Finally, the obtained DLS results illustrated that the above stated values indicate the synthesized nano-lignin particles possessed comparatively homogeneous particle size distribution and comparatively good dispersion behavior at the nano scale.³⁹

Results of XRD

X-ray Diffraction (XRD) analysis was conducted to examine whether the synthesized jute nano-lignin particles exhibited crystalline or amorphous structural characteristics. In this research, the analysis was also carried out to determine the structural characteristics of the extracted lignin and the synthesized nano-lignin particles.

In Figure 8, (x)-axis resembles X-Ray diffraction angle (2θ) and Y-axis resembles intensity of the X-Ray in CPS (count per seconds). Initially the X-Ray diffraction was 5000 count per seconds and by the increase of the diffracted angle the values were decreased, as the particles were amorphous in nature. If the particles were crystalline in nature, sharp crystalline peaks would have been obtained. The decrease of the graph was smooth and broad that indicated amorphousness.⁴⁰

Figure 8.

X-ray diffraction (XRD) of jute nano-lignin.

Generally, lignin and nano-lignin are considered amorphous materials and the indication of the experiments aligned with the test report. Figure 8 showed that in the obtained diffraction pattern, in the region of 2θ ≈ 20°–25°, a broad peak was observed. The absence of sharp crystalline peaks indicates the predominantly amorphous nature of the synthesized nano-lignin particles. This type of pattern highlighted that the sample was amorphous in nature.⁴¹

Lignin is a complex, three-dimensional and irregular structural non-crystalline biopolymer, that’s why, in XRD pattern, usually sharp diffraction peak was not generally expected. Hence, in the obtained result, the sharp peak was absent and it was aligned with the usual characteristics of lignin. This phenomenon is consistent with the amorphous structural characteristics of nano-lignin particles.⁴²

The possible presence of cellulose-related crystalline structures was examined by XRD analysis.

The contamination of cellulose was also examined by XRD analysis. In case if cellulose was found, a sharp diffraction peak would be expected in the 2θ ≈ 16° to 22° region. In this study, no sharp cellulose related crystalline peak was observed, suggesting a lower presence of crystalline cellulose components in the synthesized nano particles. Finally, in the figure of 08, due to not having any sharp crystalline peak in the diffraction pattern, it reflected that no major crystalline impurity phases were prominently present in the synthesized nano particles. It presented that the XRD results were consistent with the structural characteristics of widely reported nano-lignin particles.⁴³

All the data obtained from XRD analysis was presented in Table 4. In XRD analysis, the observed broad peak in the amorphous region and the absence of crystalline peaks supported the amorphous structural characteristics of the synthesized nano-lignin particles.

Table 4.

Values obtained in XRD for Nano-lignin.

Observations	Obtained results	Anticipated results	Clarification
Nature of the Structure	Broad peak in 2θ ≈ 20–25°	Amorphous region should be there for lignin/nano-lignin	Broad peak suggests Amorphous structure
Diffraction peak	No sharp peak	Sharp peak shouldn’t be there	Consistent with non-crystalline lignin characteristics
Nano effect	Observation of broad peak	Crystallinity will be decreased for nano particles	Suggests nano-lignin formation
Cellulose contamination	No sharp peak in 2θ ≈ 16–20°	Presence for sharp peak in 2θ ≈ 16–20° Suggests cellulose contamination	Lignin without cellulose
Impurity presence	No extra peak	No additional crystalline peak should be there	No additional crystalline impurity peak was observed

Apparent domain size from XRD

The apparent Domain Size of the synthesized nano-lignin particles was estimated using Scherrer Equation 1.

D = \frac{K λ}{β \cos θ}

(1)

Where D is the apparent domain size, K is the Shape Factor,

λ

is the X Ray wave length, β is the full width at half maximum (FWHM). Using Scherrer equation, the apparent domain size of XRD is calculated and the value is 3.5nm. This apparent value of 3.5nm falls within the generally reported value (1-5nm) ranges for amorphous lignin structures. This value is consistent with the usually reported amorphous structural characteristics of lignin-based nanoparticles.⁴⁴

Results of zeta potential

Zeta potential analysis was carried out to evaluate the surface charges and dispersion stability of the synthesized jute nano-lignin particles. In Figure 9, the X-axis represents the zeta potential (mv) values of the nano-lignin particles and the Y-axis represents the particle counts within that specific charge ranges. In this figure, a sharp and distinct single peak was observed, that situated in the -35.95mv (1 millivolt= 0.001 volt) area suggesting a comparatively uniform and well-dispersed nanoparticle system.⁴⁵

Figure 9.

Zeta potential distribution graph of nano-lignin derived from jute biomass.

The relatively high negative zeta potential values of -35.95 mv (values greater than ±30 mV generally indicates good colloidal stability) indicates comparatively stable colloidal behavior of the nano-lignin suspension, due to electrostatic repulsion among the particles, which may help reduce particle aggregation. Similar zeta potential values have also been reported in the literature for stable lignin nanoparticle dispersions.⁴⁶

Figure 10 shows the zeta potential phase plot graph. In this graph, X-axis represents time (s) and Y-axis represents phase (radian). In phase plot graph it is seen that when times increases and cross 1s, (before reaching to 1.5s) in 0 radian, the phase radian started to decrease and cross -100 radian (reaches before -120 radian). After a certain time before 2s, phase radian values again started to increase and reaches to radian 0. When time increases and reach to 3s, the radian value exposed to be the same. This phenomenon of increasing and decreasing of radian vs time indicates that the nanoparticles responded to the applied electric field and showing stable signal behavior.⁴⁷

Figure 10.

Zeta potential phase plot graph.

Table 5 presents the zeta potential values obtained from the synthesized jute nano-lignin particles. In this table the zeta potential values of -35.95mv suggests comparatively good nano-lignin dispersion stability of the nano-lignin suspension. The other important values described in the tables indicate acceptable signal quality, uniform particle distribution, and lower aggregation tendency. Overall, these data were found to be consistent with the previously reported characteristics of the stable lignin nanoparticle dispersions.⁴⁸

Table 5.

Zeta potential values of jute nano-lignin with interpretation.

S.N	Parameter	Obtained value	Unit	Reported value ranges from recent studies	Description
1	Zeta Potential	-35.95	mV	More than ±30 mV (comparatively stable dispersion)	suggests comparatively stable nano-lignin dispersion
2	Zeta Peak 1	-35.95 and single peak	mV	Single peak indicates uniform distribution	suggests uniform particle distribution
3	Conductivity	0.0199	mS/cm	Less than 1 mS/cm for lower ionic interference	lower ionic interference values suggest acceptable data reliability
4	Wall Zeta Potential	-25.46	mV	values should be in between +/- (20-30)\|mV for moderate interaction	Indicates particle’s wall interaction and aggregation tendency
5	Zeta Deviation	4.889	mV	values less than 10 mV indicates good consistency	Suggests data consistency and good measurement repeatability
6	Derived Count Rate	5074	kcps	values in between 200 to 10000 kcps	Indicates acceptable signal quality
7	Quality Factor	1.062	—	values less than 1 indicates good data quality	indicates reliable and accepted quality data

Table 6 showed the comparison values of the previous reports of the DLS and Zeta Potential Values. The DLS and Zeta Potential values found in the present research are consistent with the previously reported studies the lignin nanoparticles. According to previous reports, the DLS values were obtained in between the range of 80–250 nm, where in our present study, DLS value is found 117nm. In the literature, the Zeta Potential values were found in between the range of −25 to −35 mV, where in the present study, the ZP value is found -35 mv, which specifies the good colloidal stability. The results (DLS and ZP) represented in the present research falls within the reported value ranges of the related studies.⁴⁹

Table 6.

Comparison of the present and recent studies of the DLS and Zeta Potential.

Comparison of studies	Source	(DLS) particle size (nm)	Zeta potential (ZP) (mV)
In our research	Jute sticks	117	−35
Arun Kumar Gupta et al.⁵⁰	Wood lignin	150 to 250	-30
Qianqian Tang et al.³⁵	Different biomass	80 to 200	-25 to -35

Results of TGA (Thermo-gravimetric analysis)

Figure 11 shows the TGA (Thermo-gravimetric Analysis) report of the synthesized nano-lignin particles. In this figure, the X-axis represents the temperature (°C) and Y-axis represents the weight%. The TGA experiment was conducted within the temperature range of0°C to 600°C. the graph shows that the weight% of nano-lignin gradually decreased with increasing temperature (°C).

Figure 11.

TGA analysis report of nano-lignin.

In the initial stage up-to approximately 250°C, a slight weight loss was observed, which may be associated with the removal of absorbed moisture from the lignin nano particles. In the second stage, within the temperature range of approximately 250°C to 400°C, a substantial weight loss was observed, which might be related to the degradation of aliphatic side chains and their corresponding oxygen containing functional groups present in the nano-lignin particles.⁵¹

From the obtained TGA results, almost 52.81% weight loss was observed between 265°C and 595°C, which indicates the thermal decomposition behavior of the nano-lignin particles. The remaining residual mass was approximately (100-52.81% or 47.19%) 47.19% that may be associated with the carbon rich aromatic structure of lignin. As per the TGA Analysis report, the major thermal degradation of nano-lignin particle was initiated around 265°C, suggesting comparatively good thermal stability of the synthesized nano-lignin particles.⁵²

At higher temperature above 400°C, a slower rate of weight loss was observed, which might be associated with the gradual degradation of the aromatic structure of nano-lignin. At higher temperatures, some residual mass sustained, which indicates the carbon rich stable structure. Overall, the TGA results exhibited that the synthesized nano-lignin particles exhibited multi stage thermal degradation behavior, which is commonly consistent with the recent studies for lignin-based materials.⁵³ Table 7 showed the TGA observation for the jute nano lignin particles.

Table 7.

TGA observation for jute nano-lignin particles.

Explanation	Achieved values (°C/%)	Reported value ranges from earlier studies	Comments
Initial weight loss	At 250°C	150 to 300°C Temperature	Weight loss started due to moisture removal
Most important degradation phase	250–400°C	200–400°C Temperature	Increase temperature degrades aliphatic side chains and functional groups in nano-lignin
Total mass loss	265–595°C (around 52.81%)	40–60% weight loss	Structural decomposition for nano-lignin
Starting of thermal degradation	At 265°C	200–300°C	suggests thermal stability up-to 265°C for nano-lignin
Degradation at higher temperature	After 400°C	400°C to 600°C	Slow degradation for nano-lignin

Results of DSC

Figure 12 showed the DSC (Differential Scanning Calorimetry) analysis report of the synthesized nano-lignin particles. The X-axis of DSC report indicated temperature and Y-axis indicates the heat flow (W/g) whether the sample absorbs heat or releases. DSC analysis was carried out to evaluate the thermal transition behavior of the nano-lignin particles. In the DSC graph, several thermal transition peaks were observed at different temperature regions. At 97°C temperature, a small peak was observed, which might be associated with the moisture removal or initial thermal relaxation behavior of the nano-lignin particles. Table 8 showed the DSC Analysis report of the synthesized nano-lignin particles.⁵⁴

Figure 12.

DSC Analysis report of nano-lignin.

Table 8.

DSC analysis report of nano-lignin.

Explanation	Obtained values (°C)	Reported value ranges from published studies	Remarks
Start of thermal relaxation	At 97°C	80–120°C	Thermal relaxation and Moisture loss at this temp for nano-lignin
First main degradation peak	At 334.8°C	300–350°C	Lignin’s structural degradation
Second degradation peak	At 374.9°C	350–400°C	Degradation for aromatic network

At approximately 334.8°C temperature, a major thermal transition peak was observed, that may correspond to the primary thermal degradation region of nano-lignin structures. Besides, at the temperature of 374.9°C, another peak was observed, which might be associated with the degradation of the complex aromatic structure of lignin nano particles. This obtained DSC results represented that the synthesized nano-lignin particles underwent multiple thermal stages, which are consistent with the reported thermal behavior of lignin-based materials. Overall, the DSC analysis indicated comparatively satisfactory thermal resistance characteristics of the synthesized nano-lignin particles.⁵⁰

Conclusion

In this research, lignin was extracted from jute stick biomass using an ethanol-based organosolv method and subsequently converted into nano-lignin through a solvent–anti-solvent precipitation process. FTIR analysis supported the presence of important lignin functional groups such as hydroxyl, carbonyl, and aromatic groups after nano-lignin synthesis. SEM, XRD, and DLS analyses were conducted to evaluate the surface morphology, structural characteristics and particle size distribution of the synthesized nano-lignin particles. EDX analysis showed that carbon and oxygen were the dominant detected elements in the synthesized nano-lignin particles, which was consistent with the elemental characteristics of lignin. DLS analysis showed an average particle size of around 117 nm with uniform particle size distribution. XRD analysis indicated predominantly amorphous structural characteristics commonly reported for nano-lignin-based particles. Zeta potential analysis implied comparatively good colloidal stability of around -35 mV and dispersion behavior of the synthesized nano-lignin particles. TGA and DSC suggested multi-stage thermal degradation behavior with comparatively satisfactory thermal stability. Overall, this research demonstrated a sustainable approach for lignin extraction using an ethanol-based organosolv method and nano-lignin synthesis from jute based agro industrial biomass. The obtained characterization results were consistent with the often reported structural and physicochemical characteristics of lignin-based nanoparticles and may support further study on biomass-derived nano materials.

Footnotes

Funding

The authors received no financial support for the research, authorship, and/or publication of this article.

Declaration of conflicting interests

The authors declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

References

Abul Hasan

. Development of polyester biocomposites toughened with 40% ViscoseBamboo and 60% Caryota urens blended fibers and lignin biopolymer: characteristic analysis. Polymer Bulletin 2026; 83(5): 212. https://doi.org/10.1007/s00289-026-06289-6

Kumar

Dhakal

Næss

, et al. Application of lignin as bioasphalt in pavement engineering: a review on production, characterisation, and performance evaluation. Biomass Conversion and Biorefinery 2026; 16(7): 191. https://doi.org/10.1007/s13399-026-07116-8

Mahabaleshwar

Gaonkar

RSP

. New eco-friendly cashew nutshell liquid matrix composites: development, characterization and optimization of mechanical properties. Iranian Polymer Journal 2026: 1–25. https://doi.org/10.1007/s13726-026-01658-4

Srivorradatphisan

Ruangnarong

Sonhom

, et al. Eco-Development and Characterization of Reed-Recycled Polyester Yarns From Cyperus sp.(Cyperaceae) for Sustainable Textile Innovation. Journal of Natural Fibers 2026; 23(1): 2625778. https://doi.org/10.1080/15440478.2026.2625778

Ahmed

Al Rakib

Shahabuddin

, et al. Removal of Cr (VI) ion from aqueous solution using jute stick lignin and application of machine learning approach to determine optimal parameters. Journal of King Saud University–Science 2026; 38: 13952025. https://doi.org/10.25259/jksus_1395_2025

Akter

Alam

Mofasser

AZM

, et al. Lignocellulose-Based Nanocomposites: Processing, Characterization, and Properties. Lignocellulosic Composites. CRC Press, 2026, pp. 205–244.

Vunduk

Đurović

Kostić

, et al. The application of laccase-rich extract of spent mushroom substrates for removing lignin from jute fabric waste: a dual management approach. Scientific Reports 2025; 15(1): 12598. https://doi.org/10.1038/s41598-025-96177-2

Shoukat

Bristi

. Lignin Extraction from Jute Fabric and its Dynamic Influence on Reactive Dye Affinity. International Textile and Apparel Association Annual Conference Proceedings. Iowa State University Digital Press, 2025, vol 1. https://doi.org/10.31274/itaa.21856

Adebayo

Olanrewaju

. A Complete Review of Lignin’s Extraction, Analysis, Applications, and Future Outlook. Chemistry Africa 2025; 8(5): 1711–1741. https://doi.org/10.1007/s42250-025-01323-y

10.

Andrade

Nuñez

Henríquez-Gallegos

, et al. Interaction of Nanofibrillated cellulose with lignin nanoparticles: Effects on CNF-LNP composite properties. Carbohydrate Polymer Technologies and Applications 2025; 9: 100651. https://doi.org/10.1016/j.carpta.2024.100651

11.

Muhammad

Bairwan

Khalil

, et al. Comparative study of lignin from patchouli waste fibers and spent coffee grounds as biofillers in poly (3-hydroxybutyrate-co-3-hydroxyvalerate)-based biodegradable packaging materials. Bioresource Technology Reports 2025; 30: 102138. https://doi.org/10.1016/j.biteb.2025.102138

12.

Hasan

Hossain

Rahman

, et al. Effect of hydrolysis agitation and suspension drying temperature on the synthesis of crystalline cellulose from jute fiber. Carbohydrate Polymer Technologies and Applications 2025; 10: 100769. https://doi.org/10.1016/j.carpta.2025.100769

13.

Sharma

Hicks

Ruggiero

, et al. Extraction and analysis of carboxycellulose nanofibers from virgin plant fibers using updated TEMPO-mediated oxidation. Cellulose 2025; 32(2): 887–902. https://doi.org/10.1007/s10570-024-06328-3

14.

Hussein

Salman

. Enhancing thermo-mechanical performance of epoxy composites using alkali-treated almond shells for automotive applications. Journal of Industrial Textiles 2025; 55: 15280837251397831. https://doi.org/10.1177/15280837251397831

15.

Islam

Mozumder

. Effect of weave structures and thread densities on the cover factor and mechanical properties of cotton spandex woven fabrics. The Journal of The Textile Institute 2024; 115(3): 479–489. https://doi.org/10.1080/00405000.2023.2201106

16.

Jahan

Hossain

Das

, et al. Extraction and characterization of cellulose nanocrystals (CNCs) from jute fibers and other by-products towards a circular economy approach. Materials Circular Economy 2024; 6(1): 57. https://doi.org/10.1007/s42824-024-00149-2

17.

Rahman

Payel

MTH

Asaduzzaman

, et al. Physical properties of isolated cellulose fiber from jute and banana fiber through kraft pulping: Potential applications in packaging and regenerated fibers. SPE Polymers 2024; 5(4): 709–717. https://doi.org/10.1002/pls2.10155

18.

Salman

. Physico-Mechanical characterization property evaluation of polyvinyl butyral composites filled with macadamia nutshell. Journal of Industrial Textiles 2024; 54: 15280837241303683. https://doi.org/10.1177/15280837241303683

19.

Ortega-Sanhueza

Girard

Ziegler-Devin

, et al. Preparation and characterization of lignin nanoparticles from different plant sources. Polymers 2024; 16(11): 1610. https://doi.org/10.3390/polym16111610

20.

Hossen

Islam

Hoque

, et al. Synthesis, activation, and characterization of carbon fiber precursor derived from jute fiber. ACS omega 2024; 9(33): 35384–35393. https://doi.org/10.1021/acsomega.4c01268

21.

Gao

Sun

Duan

, et al. Controllable synthesis of lignin nanoparticles with antibacterial activity and analysis of its antibacterial mechanism. International Journal of Biological Macromolecules 2023; 246: 125596. https://doi.org/10.1016/j.ijbiomac.2023.125596

22.

Kahie

Wang

Fang

, et al. Evolution and expression analysis of the caffeoyl-CoA 3-O-methyltransferase (CCoAOMT) gene family in jute (Corchorus L.). BMC genomics 2023; 24(1): 204. https://doi.org/10.1186/s12864-023-09281-w

23.

Jagadale

Gangil

Jadhav

. Enhancing fuel characteristics of jute sticks (Corchorus Sp.) using fixed bed torrefaction process. Renewable Energy 2023; 215: 118992. https://doi.org/10.1016/j.renene.2023.118992

24.

Islam

Sarkkinen

. The Isolation and Characterization of the Lignins of Jute (Corchorus capsularis). Holzforschung 1993; 47(2): Walter de Gruyter, 123-132.

25.

Roy

TKG

Sur

Nag

. Chemistry of jute and its applications. The Jute Genome. Springer International Publishing, 2022, pp. 37–51.

26.

Syazwani

Efzan

Kok

, et al. Analysis on extracted jute cellulose nanofibers by Fourier transform infrared and X-Ray diffraction. Journal of Building Engineering 2022; 48: 103744. https://doi.org/10.1016/j.jobe.2021.103744

27.

Suman

Malhotra

Kurmi

, et al. Jute sticks biomass delignification through laccase-mediator system for enhanced saccharification and sustainable release of fermentable sugar. Chemosphere 2022; 286: 131687. https://doi.org/10.1016/j.chemosphere.2021.131687

28.

Islam

. Influence of plain, twill, and satin weave structures on the optimum colorfastness properties of reactive dyes. Trends in Sciences 2021; 18(20): 83. https://doi.org/10.48048/tis.2021.83

29.

Islam

Alam

SMM

Akter

. Influence of thermal conduction on the stretching behavior of core spandex cellulosic fabrics. Materials Today: Proceedings 2021; 38: 2563–2571. https://doi.org/10.1016/j.matpr.2020.07.682

30.

Islam

Alam

SMM

Ahmed

. Attaining optimum values of colourfastness properties of sustainable dyes on cotton fabrics. Fibres & Textiles in Eastern Europe 2020; 28(144): 110–117. https://doi.org/10.5604/01.3001.0014.3806

31.

Shariful Islam

Alam

Akter

. Investigation of the color fastness properties of natural dyes on cotton fabrics. Fibers and Textiles 2020; 27(1): 1–6.

32.

Barai

Chattopadhyay

Majumdar

. Studies on delignification in jute (Corchorus spp L.) fibre with promising lignin degrading bacterial isolates. J Environ Biol 2020; 41(4): 703–710. https://doi.org/10.22438/jeb/41/4/mrn-1252

33.

Bao

Fan

, et al. Graft modification of lignin-based cellulose via enzyme-initiated reversible addition-fragmentation chain transfer (RAFT) polymerization and free-radical coupling. International journal of biological macromolecules 2020; 144: 267–278. https://doi.org/10.1016/j.ijbiomac.2019.12.078

34.

Wang

Lou

, et al. Changes in physicomechanical properties and structures of jute fibers after tetraacetylethylenediamine activated hydrogen peroxide treatment. Journal of Materials Research and Technology 2020; 9(6): 15412–15420. https://doi.org/10.1016/j.jmrt.2020.10.096

35.

Tang

Qian

Yang

, et al. Lignin-based nanoparticles: a review on their preparations and applications. Polymers 2020; 12(11): 2471. https://doi.org/10.3390/polym12112471

36.

Ivanovska

Cerovic

Maletic

, et al. Influence of the alkali treatment on the sorption and dielectric properties of woven jute fabric. Cellulose 2019; 26(8): 5133–5146. https://doi.org/10.1007/s10570-019-02421-0

37.

Fonseca

Silva

Mendes

, et al. Jute fibers and micro/nanofibrils as reinforcement in extruded fiber-cement composites. Construction and Building Materials 2019; 211: 517–527. https://doi.org/10.1016/j.conbuildmat.2019.03.236

38.

Zhang

Shan

, et al. The KCS gene is involved in the formation of chloroplast stromules and other physiological processes in jute (Corchorus capsularis L.). Industrial Crops and Products 2019; 141: 111781. https://doi.org/10.1016/j.indcrop.2019.111781

39.

Ramakoti

Dhanagopal

Deepa

, et al. Solvent fractionation of organosolv lignin to improve lignin homogeneity: structural characterization. Bioresource Technology Reports 2019; 7: 100293. https://doi.org/10.1016/j.biteb.2019.100293

40.

Islam

. Attaining optimum strength of cotton-spandex woven fabric by apposite heat-setting temperature. Journal of The Institution of Engineers (India): Series C 2019; 100(4): 601–606. https://doi.org/10.1007/s40032-018-0478-y

41.

Shariful Islam

Alam

Akter

. Identifying the values of whiteness index, strength and weight of cotton spandex woven fabric in peroxide bleaching of different concentration. Fibers and Textiles 2019; 26(4): 96–109.

42.

Islam

Mominul Alam

. Investigation of the acoustic properties of needle punched nonwoven produced of blend with sustainable fibers. International Journal of Clothing Science and Technology 2018; 30(3): 444–458. https://doi.org/10.1108/ijcst-01-2018-0012

43.

Islam

Alam

SMM

Akter

. Identifying a suitable heat setting temperature to optimize the elastic performances of cotton spandex woven fabric. Research Journal of Textile and Apparel 2018; 22(3): 260–270. https://doi.org/10.1108/rjta-01-2018-0002

44.

Delgado-Aguilar

Oliver-Ortega

Méndez

, et al. The role of lignin on the mechanical performance of polylactic acid and jute composites. International journal of biological macromolecules 2018; 116: 299–304. https://doi.org/10.1016/j.ijbiomac.2018.04.124

45.

Manzato

Takeno

Pessoa-Junior

WAG

, et al. Optimization of cellulose extraction from jute fiber by Box-Behnken design. Fibers and Polymers 2018; 19(2): 289–296. https://doi.org/10.1007/s12221-018-1123-8

46.

Ahuja

Kaushik

Chauhan

. Fractionation and physicochemical characterization of lignin from waste jute bags: Effect of process parameters on yield and thermal degradation. International journal of biological macromolecules 2017; 97: 403–410. https://doi.org/10.1016/j.ijbiomac.2017.01.057

47.

Choudhary

Chowdhury

Singh

, et al. Morphological, histobiochemical and molecular characterisation of low lignin phloem fibre (llpf) mutant of dark jute (Corchorus olitorius L.). Applied Biochemistry and Biotechnology 2017; 183(3): 980–992. https://doi.org/10.1007/s12010-017-2477-5

48.

Choudhary

Kumar

Chowdhury

, et al. An efficient and cost effective method of RNA extraction from mucilage, phenol and secondary metabolite rich bark tissue of tossa jute (C. olitorius L.) actively developing phloem fiber. 3 Biotech 2016; 6(1): 100. https://doi.org/10.1007/s13205-016-0415-9

49.

Jahan

Rahman

JNMM

Islam

, et al. Chemical characteristics of ribbon retted jute and its effect on pulping and papermaking properties. Industrial Crops and Products 2016; 84: 116–120. https://doi.org/10.1016/j.indcrop.2016.01.054

50.

Gupta

Mohanty

Nayak

. Synthesis, characterization and application of lignin nanoparticles (LNPs). Materials Focus 2014; 3(6): 444–454. https://doi.org/10.1166/mat.2014.1217

51.

Watkins

Nuruddin

Hosur

, et al. Extraction and characterization of lignin from different biomass resources. Journal of materials research and technology 2015; 4(1): 26–32. https://doi.org/10.1016/j.jmrt.2014.10.009

52.

Shafrin

Das

Sanan-Mishra

, et al. Artificial miRNA-mediated down-regulation of two monolignoid biosynthetic genes (C3H and F5H) cause reduction in lignin content in jute. Plant molecular biology 2015; 89(4): 511–527. https://doi.org/10.1007/s11103-015-0385-z

53.

Zhang

Wang

Fan

, et al. Structural changes of lignin in the jute fiber treated by laccase and mediator system. Journal of Molecular Catalysis B: Enzymatic 2014; 101: 133–136. https://doi.org/10.1016/j.molcatb.2013.12.010

54.

Rahman

Afrin

Haque

. Characterization of crystalline cellulose of jute reinforced poly (vinyl alcohol)(PVA) biocomposite film for potential biomedical applications. Progress in Biomaterials 2014; 3(1): 23. https://doi.org/10.1007/s40204-014-0023-x