FTIR, TGA/DSC, BET, and WCA analyses of materials, as well as effects of parameters on isolating cellulose fibers from reed

Le Thi Thanh, Huong1 ; Tran, Hoang Huu2 ; Tran Nguyen Minh, An2

Published Aug 19, 2024; Updated Jan 10, 2025 on Dryad. https://doi.org/10.5061/dryad.5tb2rbpcz

Data files

Aug 19, 2024 version files 5.95 MB

Figures.zip

5.95 MB
README.md

2 KB

Dec 18, 2024 version files 57.63 KB

Data_Tables.zip

50.06 KB
README.md

7.57 KB

Dec 28, 2024 version files 59.89 KB

Data_tables.zip

49.30 KB
README.md

10.59 KB

Jan 10, 2025 version files 59.94 KB

Data_tables.zip

49.30 KB
README.md

10.64 KB

Abstract

This study focused on fabricating a cellulose aerogel for oil spill cleanup, using common reed (Phragmites australis) as the cellulose source. The process involved isolating cellulose from reed via traditional Kraft pulping, considering the effects of key factors on the isolated cellulose content. After a two-stage HP bleaching sequence, the highest cellulose content achieved was 27.2%, with 80% ISO brightness and 1% ash content under mild Kraft pulping conditions of 30% sulfidity, 20% active alkali, sustained cooking at 165°C for 3 hours, and a liquor-to-reed ratio of 8:1. Subsequently, reed-based cellulose aerogel was fabricated via a freeze-drying method using an eco-friendly NaOH/PEG aqueous solvent system, which was then modified with methyltrimethoxysilane (MTMS). The resulting aerogel exhibited remarkable characteristics, including a low density of 0.04 g/cm³, high porosity of 96%, high hydrophobicity with a water contact angle (WAC) of 141°, and a superior crude oil adsorption capacity of 35 g/g. Comprehensive characterizations of the fabricated materials, including SEM, FTIR, TGA/DSC, and WAC measurements, were evaluated. This interdisciplinary study explores the commercial promise of reed-based cellulose aerogel as a sustainable solution for oil spill cleanup efforts.

README: FTIR, TGA/DSC, BET, and WCA analyses of materials, as well as effects of parameters on isolating cellulose fibers from reed

Description of the data and file structure:

The associated supplementary files consist of data visualizations and tabular representations that provide evidence to validate the debates and outcomes, as explained in the following section. Figures 1S to 3S display the FTIR spectra of cellulose extracted from reed (RC), reed-derived cellulose aerogel (RCA), and MTMS-coated cellulose aerogel (RCA_MTMS). Figures 4S to 6S present the thermogravimetric analysis (TGA)/differential scanning calorimetry (DSC): isolated cellulose (RC), reed-based cellulose aerogel (RCA), and MTMS-coated cellulose aerogel (RCA_MTMS). Figures 7S to 8S show the BET results for two types of cellulose aerogel: reed-based cellulose aerogel (RCA) and MTMS-coated cellulose aerogel (RCA_MTMS). Figures 9S to 10S depict the water contact angles (WCA) for both the cut and external surfaces of RCA (recycled concrete aggregate). Tables 1S to 4S display the impacts of Kraft pulping parameters, such as sulfidity, active alkali, L:W ratio, and cooking time, on the isolation of cellulose fibers.

Figure 1S: The FTIR spectrum of isolated cellulose from reed (RC) – Shows the characteristic peaks associated with cellulose isolated from reed feedstock.
Figure 2S. The FTIR spectrum of reed-based cellulose aerogel (RCA) - Shows the characteristic peaks associated with cellulose aerogel.
Figure 3S. The FTIR spectrum of MTMS-coated cellulose aerogel (RCA_MTMS) - Shows the most significant peaks in MTMS-coated cellulose. aerogel.
Figure 4S. The TGA/DSC results of isolated cellulose (RC) – The thermogravimetric analysis (TGA)/differential scanning calorimetry (DSC) results of the isolated cellulose are presented.
Figure 5S. The TGA/DSC of reed-based cellulose aerogel (RCA) - The Thermal gravimetric analysis (TGA)/differential scanning calorimetry (DSC) results of cellulose aerogel are presented.
Figure 6S. The TGA/DSC of MTMS-coated cellulose aerogel (RCA_MTMS) - The Thermal gravimetric analysis (TGA)/differential scanning calorimetry (DSC) results MTMS-coated cellulose aerogel are presented.
Figure 7S. The BET results of reed-based cellulose aerogel (RCA) – The pore volume and pore size distribution of the reed-based cellulose aerogel are presented.
Figure 8S. The BET results of MTMS-coated cellulose aerogel (RCA_MTMS) – The pore volume and pore size distribution of the MTMS-coated cellulose aerogel are presented.
Figure 9S. WCA of RCA’s cut surface – The water contact angle of the reed-based cellulose aerogel was measured on the cut surface.
Figure 10S. WCA of RCA’s external surface – The water contact angle of the reed-based cellulose aerogel was measured on the external surface.
Table 1S. Effect of sulfidity on isolated cellulose – Sulfidity is a key variable in Kraft pulping that influences the efficiency of the pulping process and the quality of the isolated cellulose, making it an important parameter to investigate.
Table 2S. Effect of active alkali on isolated cellulose – Active alkali (AA), consisting of NaOH and Na₂S, serves as the active agent in Kraft pulping, making it an essential parameter to investigate.
Table 3S. Effect of L:W ratio on isolated cellulose – The liquid-to-solid ratio needs to be carefully controlled as it affects the diffusion of chemicals into materials containing cellulose, lignin, hemicellulose, and other components, making it a critical parameter to investigate.
Table 4S. Effect of cooking time on isolated cellulose – Cooking time affects cellulose degradation, influencing the yield and quality of the isolated cellulose, making it a critical parameter to investigate.

We have submitted our raw data in the file 'Data_Tables.zip,' which contains four Excel files documenting the entire cooking process of reed material. The results are presented in the following four files:

Effect of sulfidity on isolated cellulose.xlsx: Sulfidity is a key variable in Kraft pulping that influences the efficiency of the pulping process and the quality of the isolated cellulose;
Effect of active alkali on isolated cellulose.xlsx: Active alkali (AA), consisting of NaOH and Na₂S, serves as the active agent in Kraft pulping;
Effect of L:Q ratio on isolated cellulose.xlsx: The liquid-to-solid ratio needs to be carefully controlled as it affects the diffusion of chemicals into materials containing cellulose, lignin, hemicellulose, and other components;
Effect of cooking time on isolated cellulose.xlsx: Cooking time affects cellulose degradation, influencing the yield and quality of the isolated cellulose.

Descriptions

Effect of sulfidity on isolated cellulose

Entry: The number of the experiment, ranging from 1 to 4.
Reed chips: The constant feedstock of 0.5 kg used in Kraft pulping for cellulose isolation (kg).
AA% (active alkali percentage): The constant active alkali percentage of 0.2%, calculated based on the Na₂O equivalent in NaOH and Na₂S (%).
- NaOH: The amount of NaOH, measured in kilograms (kg).
- Na₂S: The amount of Na₂S, measured in kilograms (kg).
Sulfidity (%): The percentage of sulfidity, which was varied from 10% to 35%.
L:W ratio: The ratio of pulping liquor (kg) to the oven-dry weight of reed chips (kg). In this case, the L:W ratio is constant at 10:1.
Temperature: The cooking temperature (°C), which is set constant at 165°C.
Cooking time: The duration of cooking the reed chips (in hours), set constant at 2.5 hours in this case.
% Isolated cellulose: The percentage yield of purified cellulose isolated after cooking reed chips.

Effect of active alkali on isolated cellulose

Entry: The number of the experiment, ranging from 1 to 4.
Reed chips: The constant feedstock of 0.5 kg used in Kraft pulping for cellulose isolation (kg).
AA% (active alkali percentage): The constant active alkali percentage of 0.2%, calculated based on the Na₂O equivalent in NaOH and Na₂S (%), which was varied from 10% to 25%.
- NaOH: The amount of NaOH, measured in kilograms (kg).
- Na₂S: The amount of Na₂S, measured in kilograms (kg).
Sulfidity (%): The sulfidity percentage was set constant at 30%, based on the best value observed in previous experiments on the effect of sulfidity on isolated cellulose.
L:W ratio: The ratio of pulping liquor (kg) to the oven-dry weight of reed chips (kg). In this case, the L:W ratio is constant at 10:1.
Temperature: The cooking temperature (°C), which is set constant at 165°C.
Cooking time: The duration of cooking the reed chips (in hours), set constant at 2.5 hours in this case.
% Isolated cellulose: The percentage yield of purified cellulose isolated after cooking reed chips.

Effect of L.Q ratio on isolated cellulose

Entry: The number of the experiment, ranging from 1 to 4.
Reed chips: The constant feedstock of 0.5 kg used in Kraft pulping for cellulose isolation (kg).
AA%: The active alkali percentage, calculated based on the Na₂O equivalent in NaOH and Na₂S (%), was set constant at 15%, based on the best value observed in previous experiments on the effect of active alkali on isolated cellulose.
- NaOH: The amount of NaOH, measured in kilograms (kg).
- Na₂S: The amount of Na₂S, measured in kilograms (kg).
Sulfidity (%): The sulfidity percentage was set constant at 30%, based on the best value observed in previous experiments on the effect of sulfidity on isolated cellulose.
L:W ratio: The ratio of pulping liquor (kg) to the oven-dry weight of reed chips (kg). In this case, the ratios used were L:W = 6:1, L:W = 8:1, L:W = 10:1, and L:W = 12:1.
Temperature: The cooking temperature (°C), which is set constant at 165°C.
Cooking time: The duration of cooking the reed chips (in hours), set constant at 2.5 hours in this case.
% Isolated cellulose: The percentage yield of purified cellulose isolated after cooking reed chips.

Effect of cooking time on isolated cellulose

Entry: The number of the experiment, ranging from 1 to 4.
Reed chips: The constant feedstock of 0.5 kg used in Kraft pulping for cellulose isolation (kg).
AA%: The active alkali percentage, calculated based on the Na₂O equivalent in NaOH and Na₂S (%), was set constant at 15%, based on the best value observed in previous experiments on the effect of active alkali on isolated cellulose.
- NaOH: The amount of NaOH, measured in kilograms (kg).
- Na₂S: The amount of Na₂S, measured in kilograms (kg).
Sulfidity (%): The sulfidity percentage was set constant at 30%, based on the best value observed in previous experiments on the effect of sulfidity on isolated cellulose.
L:W ratio: The ratio of pulping liquor (kg) to the oven-dry weight of reed chips (kg). In this case, L:Q was set constat at 8:1, based on the best value observed in previous experiments on the effect of L:W ratio on isolated cellulose.
Temperature: The cooking temperature (°C), which is set constant at 165°C.
Cooking time: The duration of cooking the reed chips (in hours), was varied from 2 hours to 3.5 hours.
% Isolated cellulose: The percentage yield of purified cellulose isolated after cooking reed chips.

Version changes

23-Dec-2024:

Deleted one unnecessary first column from the two Sulfidity columns (%) in the "Effect of Sulfidity on Isolated Cellulose" sheet.
Edited all AA (%) columns in the "Effect of L:W Ratio on Isolated Cellulose" sheet and the "Effect of Cooking Time on Isolated Cellulose" sheet to a fixed value of 15%, as this represents the best AA percentage determined from previous experiments on the "Effect of Active Alkali on Isolated Cellulose."
Revised all instances of "L/Q" to "L:Q" for consistency with the manuscript.
Corrected spelling errors and formatting in all four sheets of the Data-Tables.
Corrected "DTA" to "TGA/DSC" in the "FTIR, BET, and TGA/DSC analyses of materials, as well as the effects of parameters on isolating cellulose fibers from reed" to ensure consistency with the manuscript
Rewrote the descriptions of "FTIR, BET, and TGA/DSC analyses of materials, as well as the effects of parameters on isolating cellulose fibers from reed" to ensure greater clarity, completeness, and consistency with both the manuscript and the Supporting information.