DOI: 10.5061/dryad.5tb2rbpcz
title: FTIR, TGA/DSC, BET, and WCA analyses of materials, as well as effects of parameters on isolating cellulose fibers from reed

description: 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.
description: Conducted experimental chemistry at a scaled-up level, collected
 data, tested physical and chemical properties, and applied the results to
 crude oil absorption.
description: # 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. **23-Dec-2024:**  * Corrected "DTA" to
 "TGA/DSC" in the "Supporting Information" to ensure
 consistency with the manuscript