Qualitative characterization of solid residue from hydrothermal liquefaction of biomass using thermochemolysis and stepwise pyrolysis-gas chromatography-mass spectrometry

Madsen, René B.; Jensen, Mads Mørk; Glasius, Marianne

doi:10.1039/c7se00357a

Cited by 11 publications

(14 citation statements)

References 36 publications

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“…HTL resulted in a clear decrease in the abundance of pyrolysates produced from native biomass molecules (carbohydrates, lignols and hydroxycinnamic acids). An almost complete disappearance of native lignin structure and hydroxycinnamic acids after HTL has been reported for Protobind 1000 and Lignoboost lignins. , An increased abundancy of aromatic nitrogen pyrolysates was observed after HTL, which requires further investigation, yet, could be a result of reaction between protein and lignocellulose …”

Section: Resultsmentioning

confidence: 79%

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Hydrothermal Liquefaction of Enzymatic Hydrolysis Lignin: Biomass Pretreatment Severity Affects Lignin Valorization

Jensen

Djajadi

Torri

et al. 2018

ACS Sustainable Chem. Eng.

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Section: Resultsmentioning

confidence: 79%

“…The results are ambiguous when calculating the o / p -ratio using only the o -alkyl phenolics and their corresponding p -isomer ( o / p -subgroup). The near equal o / p -subgroup ratios after HTL could be a result of loss of alkyl substituents followed by both p - and o -directed repolymerization after HTL …”

Section: Resultsmentioning

confidence: 99%

Hydrothermal Liquefaction of Enzymatic Hydrolysis Lignin: Biomass Pretreatment Severity Affects Lignin Valorization

Jensen

Djajadi

Torri

et al. 2018

ACS Sustainable Chem. Eng.

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“…This may be due to the presence of fatty amides in bio-crudes from protein-rich feedstocks or the presence of water. 26 which may explain the relatively large deviation for pine. The diversity of HTL bio-crudes also means that a variety of phenolics will be abundant in different amounts, which will vary in their specific absorptivities.…”

Section: Pls-r Was Performed To Confirm the Correlation Observed Betwmentioning

confidence: 97%

Rapid Determination of Water, Total Acid Number, and Phenolic Content in Bio-Crude from Hydrothermal Liquefaction of Biomass using FT-IR

et al. 2018

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This paper investigates the use of Fourier-transform infrared spectroscopy (FT-IR) for quantitative analysis of bio-crudes from hydrothermal liquefaction (HTL) of biomass. HTL is a versatile process rendering virtually all biomasses suitable for conversion into bio-crude and side-streams. However, continuous processes require rapid analytical methods applicable to highly diverse bio-crudes. Bio-crudes were obtained from two different continuous HTL reactors (lab scale and pilot scale) and in some cases recirculation of water. The bio-crudes originated from a diverse range of feedstocks including lignocellulosics (pine, Miscanthus), microalgae (Spirulina, Chlorella vulgaris), and residues (sludge, dried distillers grains with solubles). Quantitative analysis of water content, total acid number, and total content of phenolics was performed using FT-IR. Principal component analysis indicated a potential correlation between quantitative measurements and FT-IR. Partial least squares regression was used to develop predictive models that performed well considering the high diversity of the bio-crudes. The content of phenolics was 83.1-254.6 mg g-1 (gallic acid equivalent) and model calibration was good (RMSE = 19.7, slope = 0.81, y-exp = 81.2%). A diverse set of test samples were subjected to the models. The relative difference for measured and predicted phenolic content was generally < 15%. Total acid numbers (TAN) were 7-98 mgKOH g-1 and model calibration was found to be satisfactory considering the titration method used (RMSE = 18.5, slope = 0.53, y-exp = 52.6%). The relative difference for measured and predicted TAN was generally < 20%. The water content (Karl Fischer titration) was 1-24 % and model calibration was very good (RMSE = 2.0, slope = 0.93, y-exp = 92.6%). The water content was generally predicted within 1.5% and the relative difference for measured and predicted water content was large (2.7-16.6%) due to the small values. All models included samples that deviated and could be considered outliers, however, their deviations were explained from their composition and retained in the models. Overall, the results show the potential of FT-IR as a universal technique to obtain rapid quantitative results from a variety of bio-crudes processed using different reactors.

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“…25,30 Although stepwise pyrolysis has been used for some time, 24,26,31,32 recent advances in pyrolizer instruments have made stepwise pyrolysis more accessible. 11,28,[33][34][35] Low-temperature steps remove volatile and/or extractable compounds while higher-temperature steps degrade insoluble carbonaceous compounds into smaller molecular pieces by breaking bonds at different temperatures depending on the bond type or strength. 32 Using IOM from carbonaceous chondrites and Type III kerogen, Mimura and colleagues showed how stepwise pyrolysis GC/MS is an effective method for detecting both thermally labile and refractory fractions.…”

Section: Introductionmentioning

confidence: 99%

Comparison of stepwise and single-step pyrolysis GC/MS for natural complex macromolecular organic matter

2022

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Pyrolysis gas chromatography-mass spectrometry (GC/MS) is a useful technique for the analysis of complex organic matter. However, pyrolysis temperatures must be carefully chosen in order to maximize the information obtained and, in parallel, minimize byproducts. One solution to accomplish this is the stepwise pyrolysis method, which has been employed to analyze complex mixtures of natural samples. Here we compared the stepwise pyrolysis method to a suite of single-step pyrolysis runs using the same temperatures using a humic acid standard sample, in order to evaluate the advantage of the stepwise pyrolysis method. In addition, we conducted in-situ heating experiments of the humic acid under infrared microspectroscopy to observe changes in the functional groups during the stepwise pyrolysis process. Results showed that O-bearing components were released at relatively low temperatures whereas aromatic components were released at higher temperatures, indicating that the stepwise method effectively separates labile and refractory fractions. As such, the stepwise method would be useful for analyzing limited amounts of samples such as for extraterrestrial materials as well as for payload instruments onboard space missions.

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Qualitative characterization of solid residue from hydrothermal liquefaction of biomass using thermochemolysis and stepwise pyrolysis-gas chromatography-mass spectrometry

Abstract: Hydrothermal liquefaction of biomass produces solid residue (char) as an unwanted byproduct, which was characterized using advanced techniques in order to understand its composition and formation reactions.

Cited by 11 publications

References 36 publications

Hydrothermal Liquefaction of Enzymatic Hydrolysis Lignin: Biomass Pretreatment Severity Affects Lignin Valorization

Hydrothermal Liquefaction of Enzymatic Hydrolysis Lignin: Biomass Pretreatment Severity Affects Lignin Valorization

Rapid Determination of Water, Total Acid Number, and Phenolic Content in Bio-Crude from Hydrothermal Liquefaction of Biomass using FT-IR

Comparison of stepwise and single-step pyrolysis GC/MS for natural complex macromolecular organic matter

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