Investigation of functional group changes in biomass during slow pyrolysis using synchrotron based infra-red microspectroscopy and thermogravimetry-infra-red spectroscopy

Parihar, Anurag; Sripada, Pramod; Bambery, Keith R.; Garnier, Gil; Bhattacharya, Sankar

doi:10.1016/j.jaap.2017.07.010

Cited by 34 publications

(7 citation statements)

References 26 publications

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“…When the temperature reaches 350 C, absorption peaks at 3950-3600 cm À1 and 1000-800 cm À1 are generated, corresponding to the vibration of the O H and C H bonds, respectively. [32][33][34] In addition, the intensity of the absorption peaks decreases rapidly after 380 C, which is consistent with the DTG curve of sample IL/AA-3 in Figure 4c. The positions of each absorption peak and the possible types of functional groups are shown in Table 3.…”

Section: Thermal Stability Of Modified Pmesupporting

confidence: 86%

Flame retardant polyurethane microbubble elastomer based on ionic liquid/ammonium polyphosphate/aluminum hypophosphite ternary flame retardant system

Liu,

Gao,

Liu

et al. 2024

J of Applied Polymer Sci

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To develop a highly efficient flame retardant system for polyurethane microbubble elastomer (PME), a phosphate‐based ionic liquid (IL) 1‐methyl‐3‐(dioxyphosphoryl)‐propyl imidazole bromide was synthesized, and then combined with ammonium polyphosphate (APP) and aluminum hypophosphate (ALHP) to form a ternary flame retardant system, which shows excellent synergistic flame retardancy and plays an important role in both gas phase and condensed phase flame retardancy. Compared with pure PME, the limiting oxygen index of flame retardant PME with 6 wt% IL and 15 wt% APP/ALHP increased from 20.25% to 29.25%, the char yields is increased by 13 times, and the heat release rate, total heat release rate, mass loss rate, and smoke production rate are reduced by 74%, 19%, 67%, and 22%, respectively. Ignition time increased from 9 s to 19 s, and extinguishing time increased from 295 s to 573 s. At the same time, the addition of IL promoted the dispersion and compatibility of APP/ALHP in the PME matrix and improved the mechanical properties. In addition, IL also shows potential in antistatic modification, providing the possibility for materials to meet both flame retardant and antistatic requirements.

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Section: Thermal Stability Of Modified Pmesupporting

confidence: 86%

Flame retardant polyurethane microbubble elastomer based on ionic liquid/ammonium polyphosphate/aluminum hypophosphite ternary flame retardant system

Liu,

Gao,

Liu

et al. 2024

J of Applied Polymer Sci

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“…Similar changes are reported and discussed in detail elsewhere in the literature. 17 Lower concentration of acid (up to 0.1 M) was observed to stabilize certain functional groups of biomass up to 500 °C. The O−H (∼3400 cm −1 ) and C−H (∼2900 cm −1 ) functional groups in the raw biomass substantially diminished at a temperature higher than 400 °C (see Supporting Information Figure S4) but were observed after 400 °C in the acid-treated biomass at 0.05 and 0.1 M acid concentration (Figure 11a,b).…”

Section: Resultsmentioning

confidence: 95%

“…Changes in spectral features observed for raw biomass during thermal breakdown are presented in Supporting Information Figure S4. Similar changes are reported and discussed in detail elsewhere in the literature …”

Section: Resultsmentioning

confidence: 99%

“…15 However, that study does not illustrate the chemical changes that occur in the acid-treated feedstock. Similarly, other studies elucidate the functional group changes in woody 16,17 and algal biomass 18 during thermochemical conversion but not for the feedstock treated with acid. Mayes et al used quantum mechanics calculations to illustrate the reaction pathways involved in the thermochemical conversion (pyrolysis) of glucose, 19 and Jadhav et al determined the reaction rates to investigate the intermediates during glucose conversion to furans.…”

Section: Introductionmentioning

confidence: 99%

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Synchrotron-Based Infra-Red Spectroscopic Insights on Thermo-Catalytic Conversion of Cellulosic Feedstock to Levoglucosenone and Furans

2019

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Thermo-catalytic conversion of cellulosic feedstock, such as lignocellulose, to platform chemicals offers a renewable alternative to fossil-based chemicals. Mechanistic insights behind thermochemical conversion of lignocellulose would facilitate thermo-catalytic process development for bio-based chemicals. This study employed synchrotron-based Fourier transform infrared (FTIR) microspectroscopy to investigate chemical changes in acid-catalyzed cellulose and lignocellulose and glucose during pyrolysis. Major changes in glucose occurred at 200 °C, where it underwent reactions including ring opening and tautomerization. Acid treatment did not change the molecular structure of cellulose but disrupted the lignocellulose network. The observed synchrotron FTIR spectral features provided evidence for acceleration of catalytic dehydration of cellulose and lignocellulose to levoglucosenone and furans. Catalytic passivation of alkali and alkaline earth metals in lignocellulose was also observed at low acid concentration.

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“…44 The release of volatiles during pyrolysis is known to lead to micropores in the material. 45,46 Large mesopores and macropores, present in the pure carbon matrix, are due to interstices formed by clustering of primary particles to aggregates. Compared with the pure materials, the iron oxide-loaded composites contain small mesopores, less micropores, but no macropores.…”

Section: Discussionmentioning

confidence: 99%

Tuning the Properties of Iron-Doped Porous Graphitic Carbon Synthesized by Hydrothermal Carbonization of Cellulose and Subsequent Pyrolysis

et al. 2019

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The applied pyrolysis temperature was found to strongly affect composition, structure, and oxidation behavior of pure and iron oxide nanoparticle (NP)-loaded carbon materials originating from hydrothermal carbonization (HTC) of cellulose. A strong loss of functional groups during pyrolysis at temperatures beyond 300 °C of the HTC-derived hydrochars was observed, resulting in an increase of the carbon content up to 95 wt% for the carbon materials pyrolyzed at 800 °C and an increase of the specific surface area with a maximum of 520 m 2 g –1 at a pyrolysis temperature of 600 °C. Devolatilization mainly took place in the range from 300 to 500 °C, releasing light pyrolysis gases such as CO, CO 2 , H 2 O and larger oxygen-containing molecules up to C 11 . The presence of iron oxide NPs lowered the specific surface areas by about 200 m 2 g –1 and resulted in the formation of mesopores. For the iron oxide-containing composites pyrolyzed up to 500 °C, the oxidation temperature was decreased by about 100 °C, indicating tight contact between the iron oxide NPs and the carbon matrix. For higher pyrolysis temperatures, this catalytic effect of iron oxide on carbon oxidation vanished due to carbothermal reduction to iron and iron carbide, which, however, catalyzed the graphitization of the carbon matrix. Thus, the well-controlled two-step synthesis based on a biomass-derived precursor yielded stably embedded iron NPs in a corrosion-resistant graphitic carbon matrix.

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Investigation of functional group changes in biomass during slow pyrolysis using synchrotron based infra-red microspectroscopy and thermogravimetry-infra-red spectroscopy

Cited by 34 publications

References 26 publications

Flame retardant polyurethane microbubble elastomer based on ionic liquid/ammonium polyphosphate/aluminum hypophosphite ternary flame retardant system

Flame retardant polyurethane microbubble elastomer based on ionic liquid/ammonium polyphosphate/aluminum hypophosphite ternary flame retardant system

Synchrotron-Based Infra-Red Spectroscopic Insights on Thermo-Catalytic Conversion of Cellulosic Feedstock to Levoglucosenone and Furans

Tuning the Properties of Iron-Doped Porous Graphitic Carbon Synthesized by Hydrothermal Carbonization of Cellulose and Subsequent Pyrolysis

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