4.7 Article

Structural and chemical changes of sludge derived pyrolysis char prepared under different process temperatures

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Publisher

ELSEVIER
DOI: 10.1016/j.jaap.2021.105085

Keywords

Sewage sludge; Pyrolysis; Sludge-char; NMR; Raman spectroscopy; XPS

Funding

  1. Ministry of Agriculture of the Czech Republic [QK21020022]
  2. Ministry of Education, Youth and Sports of the Czech Republic
  3. EU - European Structural and Investment Funds - Operational Programme Research, Development and Education - project SPETEP [CZ.02.1.01/0.0/0.0/16_026/0008413]
  4. Phos4You project through INTERREG North West Europe Program
  5. AV 21 - Efficient energy transformation and storage
  6. [A1_FTOP_2021_004]

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Pyrolysis of sewage sludge at 400-800 degrees C showed that increasing temperature led to higher phosphate and metaphosphate content, and lower reduced P species content; higher temperature also increased sulfide content and decreased sulfate and sulfite content; the effect on nitrogen species was minimal. Raman spectroscopy and NMR revealed significant contribution of graphite and (poly) aromatic hydrocarbons to the organic structure of sludge-chars.
Sewage sludge was pyrolyzed at 400-800 degrees C to study the influence of the pyrolysis temperature on the bulk and structural properties of the resulting sludge-chars. For this purpose, sludge-chars were subjected to proximate and ultimate analyses and the textural and porous properties were examined by the nitrogen adsorption-desorption isotherm. Raman spectroscopy was employed to correlate the results of the structural changes of the sludge-chars obtained by conventional analysis (textural properties) and together with solid state NMR it was used to characterize the organic part of the sludge-chars. Additionally, an XPS of the chars' surfaces and inner layers of the char particles was conducted to study the phosphorus, nitrogen and sulfur speciation and its changes with regard to the change in pyrolysis temperature and the depth of the char particles. Raising the pyrolysis temperature increased the relative content of phosphates and metaphosphates and decreased the reduced P species relative content. Sulfur speciation analysis revealed an increase in sulfides content and a decrease in sulfates and sulfites content as the temperature was raised. The influence of the temperature on N speciation was marginal. The NMR and Raman spectroscopy results showed a significant contribution of graphite and (poly) aromatic hydrocarbons and a negligible contribution of the carbonyl groups to the structure of the organic part of sludge-chars. The increase in the pyrolysis temperature increased the content of (poly)aromatic hydrocarbons over the total carbon content, revealing its contribution to the porosity evolution. This is in good correlation with the microporosity and surface area analyses. Regarding the sludge-char potential soil application, the results may help to predict and better understand the sludge-char stability and N and P plant availability.

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