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  • 1.
    Kozyatnyk, Ivan
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Valorization of Humic Acids by Hydrothermal Conversion into Carbonaceous Materials: Physical and Functional Properties2019In: ACS Sustainable Chemistry and Engineering, E-ISSN 2168-0485, Vol. 7, no 2, p. 2585-2592Article in journal (Refereed)
    Abstract [en]

    Humic acids (HAs) represent an economic and environmental challenge in water treatment, as they have the propensity to foul membranes and create toxic byproducts when interacting with chlorine. To overcome this, HAs were submitted to hydrothermal carbonization to convert them into an easy to remove, valuable carbon material. The result was a carbonaceous material which was easy to filter/dewater compared to HAs with a char yield of 49 +/- 1.8 wt %, and with 46.6 1.4 wt % ending up in the water phase, 2.2 +/- 0.2 wt % in the tar, and the rest in the gaseous fraction. The molecular weight distribution of the organic matter in the water pre-and post-HTC indicated that the structure was broken into several different fragments with a lower molecular weight than that initially present. Physicochemical analysis of the material via elemental analysis, X-ray photoelectron spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy, and solid-state nuclear magnetic resonance indicated that under hydrothermal carbonization, the aromatic structure of HAs condensed. Carboxylic acids groups were also lost from the surface of HAs, with ether and alcohols increasing because of their loss. The morphology of the obtained material had an amorphous macrostructure consisting of many smaller light lamellar carbon fragments. Finally, the hydrothermal treatment increased the surface area from 0.4 to 103.0 m(2) g(-1).The porosity is located in the mesoporous range of 10-80 nm with a maximum peak at 50 nm.

  • 2.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, Callaghan, Australia.
    Donne, Scott W.
    Nitrogen Doped Heat-Treated and Activated Hydrothermal Carbon: examination of Electrochemical Performance Using Step Potential Electrochemical Spectroscopy2018In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 165, no 11, p. A2840-A2848Article in journal (Refereed)
    Abstract [en]

    Step potential electrochemical spectroscopy (SPECS) has been applied to nitrogen-doped and non-doped hydrothermal carbons that have been activated or heat-treated at a range of temperatures. The highest surface area achieved was 422 m(2).g(-1) under heat-treatment at 600 degrees C, and 2275 m(2).g(-1) using H3PO4 chemical activation at 800 degrees C. The heat-treated series reported a maximum capacitance of 84 F.g(-1) at 10 mV.s(-1), whereas the activated series had a maximum capacitance of 306 F.g(-1) at 10 mV.s(-1) . SPECS analysis revealed that pseudo-capacitance for the hydrothermal carbon doped with nitrogen was interlinked with the degree of oxygen functionality, and that decreasing the oxygen content of the surface increased the pseudo-capacitance contribution from nitrogen. Pseudo-capacitance also increased with activation from the incorporation of phosphate groups; however, the nitrogen-doped hydrothermal carbons displayed minimal double-layer capacitance (60.6 F.g(-1) at 10 mV.s(-1)) despite having reasonable surface areas (1500-1600 m(2).g(-1)).

  • 3.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, Callaghan, NSW 2308, Australia.
    Dose, Wesley M.
    Allen, Jessica A.
    Donne, Scott W.
    Nitrogen doped heat treated and activated hydrothermal carbon: NEXAFS examination of the carbon surface at different temperatures2018In: Carbon, ISSN 0008-6223, E-ISSN 1873-3891, Vol. 128, p. 179-190Article in journal (Refereed)
    Abstract [en]

    Hydrothermal carbons have been shown to have controllable surface functionalization through various post-treatment techniques, which indicates these materials may be tuned for specific applications. For this reason, Near Edge X-ray Absorption Fine Structure (NEXAFS) studies have been conducted on a series of nitrogen doped and non-doped heat treated and activated hydrothermal carbons to further understand the changes in surface functionality with treatment. The NEXAFS carbon K-edge spectrum of the non-doped samples displayed a loss of oxygen functionalities (C=O and C-OH) as well as the furan ring structure with increasing temperature, while C=C bonds from graphitic groups increased. This effect was amplified further upon the addition of phosphoric acid (H3PO4) during activation. The doped hydrothermal carbons displayed similar functionality to the non-doped, although the effect of both heat treatment and activation was diminished. The nitrogen K-edge displayed characteristic peaks for pyridine and imines/amides, with pyrroles located under the broad ionization step. This work represents the first time a series of heat treated and activated hydrothermal carbons have been examined via NEXAFS spectroscopy. Additionally, difference analysis has been applied to the NEXAFS spectra to obtain a deeper understanding in the changes in surface functionality, a previously unused technique for these materials. 

  • 4.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, Callaghan, NSW 2308, Australia.
    Ferguson, Adam
    Donne, Scott W.
    Influence of ammonium salts and temperature on the yield, morphology and chemical structure of hydrothermally carbonized saccharides2019In: SN Applied Sciences, ISSN 2523-3963, E-ISSN 2523-3971, Vol. 1, no 1, article id 54Article in journal (Refereed)
    Abstract [en]

    In this work, the influence of (NH4)(2)SO4 and (NH4)(2)HPO4 as well as temperature is examined on the hydrothermal carbonization of glucose, fructose and sucrose. Increasing the temperature from 160 to 220 degrees C increased the yield of hydrothermal carbon for each saccharide for the (NH4)(2)SO4 solution, whereas (NH4)(2)HPO4 produced a yield that was independent of temperature. The addition of (NH4)(2)SO4 increased the yield obtained at 220 degrees C by 4.27, 7.03 and 2.01 wt% for glucose, fructose and sucrose over the baseline salt free solution, respectively. (NH4)(2)SO4 also increased the quantity of acid produced and the average size of the hydrothermal carbon spheres. Conversely, (NH4)(2)HPO4 produced carbon structures consisting of interlocked spherical shapes and produced almost no acidic products. XPS analysis revealed that (NH4)(2)SO4 incorporated nitrogen and sulfur into the hydrothermal structure, while (NH4)(2)HPO4 only allowed nitrogen to be incorporated. It was assessed that NH4(+) enhances the production of hydrothermal carbon, except in the presence of PO43-, which prevents the reaction from effectively forming hydrothermal carbon and organic acids. [GRAPHICS] .

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  • 5.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, Callaghan, Australia.
    Forghani, Marveh
    Dose, Wesley M.
    Allen, Jessica A.
    Donne, Scott W.
    Influence of counter ions of ammonium for nitrogen doping and carbon properties in hydrothermal carbonization: characterization and supercapacitor performance2021In: Materials Advances, E-ISSN 2633-5409, Vol. 2, no 1, p. 384-397Article in journal (Refereed)
    Abstract [en]

    Ammonium has been successfully utilized to nitrogen dope carbon structures via hydrothermal carbonization, although the influence of different attached counter ions (anions) on the resultant carbon physicochemical properties and electrochemical performance has not been examined before. Four different counter ions (SO42-, PO43-, Cl-, and Fe(SO4)(2)) attached to ammonium were seen to influence the hydrothermal reaction, nitrogen incorporation levels, physicochemical properties, activation ability and supercapacitor performance. For instance, nitrogen K-edge NEXAFS found differences in the levels of pyridinic and pyrrolic groups with PO43- incorporating predominately pyridinic nitrogen groups. PO43- also achieved the highest surface area (2132.6 m(2) g(-1)), however this material was unstable as a supercapacitor, losing almost 50% of its performance over 500 cycles. SO42- resulted in the highest level of nitrogen incorporation (5.53 at%) and hydrothermal yield (45.5%), while Fe(SO4)(2)(2-) resulted in the lowest (2.92 at%). However, Fe(SO4)(2)(2-) produced unique flower like structures not seen in any of the other anions. Cl- produced the highest performing material, achieving 190 F g(-1) at 10 mV s(-1) in 1 M KOH and had moderate nitrogen incorporation (3.42 at%). Overall, this study indicates that the anion has substantial influence on the physicochemical properties of the material, allowing an additional level of tailoring.

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  • 6.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, NSW, Callaghan, Australia.
    Kozyatnyk, Ivan
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Figueira, Joao
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Carlborg, Markus
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Rosenbaum, Erik
    MTC-Miljötekniskt Center AB, Dåva Energiväg 8, Umeå, Sweden.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Self-generation of low ash carbon microspheres from the hydrothermal supernatant of anaerobic digestate: Formation insights and supercapacitor performance2021In: Chemical Engineering Journal Advances, E-ISSN 2666-8211, Vol. 6, article id 100097Article in journal (Refereed)
    Abstract [en]

    This work provides the first observations of and insights into the self-generation of carbon microspheres from the supernatant after hydrothermal carbonization of anaerobic digestate has been completed and the hydrochar removed. Solid State NMR and XPS revealed that the carbon microspheres were comprised of decomposed fragments of proteins, carbohydrates and lignin. The carbon microspheres were significantly lower in ash content (3.1%), compared to the hydrothermal solid (41.2%) and precursor (25.2%) and their formation reduced the total organic carbon load of the supernatant. The low ash content allowed them to be easily activated, achieving a surface area of 1711.0 m2 g−1, compared to 51.4 m2 g−1 for the activated hydrothermal solid and 12.8 m2 g−1 for the activated precursor. The microcarbon spheres achieved a specific capacitance from cyclic voltammetry of 86 F g−1 at 100 mV s−1 to 176 F g−1 at 1 mV s−1, while the gravimetric capacitance was 42 F g−1 at 25 A g−1 and 140 F g−1 at 0.5 A g−1 in 0.5 M Li2SO4 and a 1.8V potential window. Overall, this study highlights the importance of exploring this new product and its valorisation potential for the hydrothermal carbonization of ash-rich precursors.

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  • 7.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, NSW, Callaghan, Australia.
    Matsakas, Leonidas
    Biochemical Process Engineering, Division of Chemical Engineering, Department of Civil, Environmental and Natural Resources Engineering, Luleå University of Technology, Luleå, Sweden.
    Figueira, Joao
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kozyatnyk, Ivan
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Occupational and Environmental Medicine Center, Department of Clinical and Experimental Medicine, Linköping University, Linköping, Sweden.
    Rova, Ulrika
    Biochemical Process Engineering, Division of Chemical Engineering, Department of Civil, Environmental and Natural Resources Engineering, Luleå University of Technology, Luleå, Sweden.
    Christakopoulos, Paul
    Biochemical Process Engineering, Division of Chemical Engineering, Department of Civil, Environmental and Natural Resources Engineering, Luleå University of Technology, Luleå, Sweden.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Impact of temperature and residence time on the hydrothermal carbonization of organosolv lignin2022In: Journal of Analytical and Applied Pyrolysis, ISSN 0165-2370, E-ISSN 1873-250X, Vol. 166, article id 105623Article in journal (Refereed)
    Abstract [en]

    Herein, we have investigated how pure lignin extracted from birch and spruce via a hybrid organosolv/steam explosion method reacts under hydrothermal carbonization (HTC) to produce hydrochar, a product that has found applications in environmental remediation, energy storage and catalysis. We subjected thirteen lignin samples obtained from birch and spruce under different extraction conditions to HTC at 260 ℃ for four hours. The yield of hydrochar varied between the different extraction conditions and source, although no clear correlation between extraction conditions and yield could be observed. For instance, lignin from birch pretreated in 60%v/v ethanol for 15 min resulted in a hydrochar yield of 39 wt%. Increasing the time to 30 and 60 resulted in a hydrochar yield of 27 wt% and 23 wt%, respectively. This suggested that small changes in the organosolv reaction conditions might produce highly structurally different lignin, resulting in the difference in HTC yield. Thus, we chose a subset of four lignin samples to investigate in-depth, subjecting these samples to a range of hydrothermal reaction temperatures and residence times. Solid State NMR and FTIR analysis indicated that the most significant structural changes occurred below 230 ℃ resulting in the breaking of C-O- linkages. Increasing the temperature or time had minimal impact, with no further C-O- linkages broken and no changes to the ring structure of C-C groups. Size exclusion chromatography indicated that the degree of micro and macromolecules in the liquid product varied significantly with lignin source and HTC reaction conditions. Overall, this study demonstrated that lignin has a large reaction range where it produces a very chemically similar solid product, with the only major difference being the yield of material. This is important for industry, as it indicates that a similar solid product can be easily achieved independently of extraction conditions allowing the HTC reaction to be tuned towards extracting the maximum benefit from products contained in the liquid.

  • 8.
    Latham, Kenneth G.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Discipline of Chemistry, University of Newcastle, Callaghan, NSW, Australia.
    Matsakas, Leonidas
    Biochemical Process Engineering, Division of Chemical Engineering, Department of Civil, Environmental and Natural Resources Engineering, Luleå University of Technology, Luleå, Sweden.
    Figueira, João
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Rova, Ulrika
    Biochemical Process Engineering, Division of Chemical Engineering, Department of Civil, Environmental and Natural Resources Engineering, Luleå University of Technology, Luleå, Sweden.
    Christakopoulos, Paul
    Biochemical Process Engineering, Division of Chemical Engineering, Department of Civil, Environmental and Natural Resources Engineering, Luleå University of Technology, Luleå, Sweden.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Examination of how variations in lignin properties from Kraft and organosolv extraction influence the physicochemical characteristics of hydrothermal carbon2021In: Journal of Analytical and Applied Pyrolysis, ISSN 0165-2370, E-ISSN 1873-250X, Vol. 155, article id 105095Article in journal (Refereed)
    Abstract [en]

    Seven different lignin samples, three from Kraft extraction and four from organosolv extraction, were subjected to hydrothermal treatment at 260℃ for four hours to assess the impact of lignin type on the physicochemical properties of the hydrothermal material. The 13C Solid state NMR, XPS, FTIR and SEM analysis revealed that the different sources of lignin and the extraction conditions created variations in the degree of syringyl and guaiacyl subunits, inter-unit bonding arrangements, morphology and surface composition. Hydrothermal carbonization appeared to “normalize” the differences between each of the lignin samples, via breaking β-O-4 or α-O-4 linkages, removal of methoxy and syringyl subunits, and creation of C–C and 4-O-5 linkages to polymerization into large 100−200 μm amorphous carbon particles. Overall, this study indicates that the source and extraction type have minimal influence on the physicochemical structure and morphology of the final hydrothermal product.

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  • 9.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boily, Jean-Francois
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Bergknut, Magnus
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Tailoring the functionality of waste materials using hydrothermal carbonization for water treatment applicationsManuscript (preprint) (Other academic)
    Abstract [en]

    Purpose:

    The material properties of carbons from hydrothermal carbonization (HTC), typically referred to as hydrochars, are crucial for hydrochar use in adsorption-related applications. More knowledge is needed on how HTC temperature is altering material properties of different wet low-cost materials and how it is affecting adsorption of contaminants. Studies systematically comparing different feedstocks and carbonization temperatures are needed, because comparisons between available studies are obstructed by the differences in reaction conditions and analysis techniques. 

    Methods: In this study, hydrochars were prepared at 180℃, 220℃, and 260℃ from fiber sludge and biosludge from a paper mill, digested sewage sludge, and horse manure. Surface properties of the raw materials and chars were characterized and the adsorption capacity of methylene blue was studied. 

    Results: The most substantial change, i.e., a decrease in the oxygen-functionalities of cellulose-rich materials (horse manure and fiber sludge), was caused by degradation of cellulose, while digested sludge types (biosludge and sewage sludge) seemed not to change substantially with the HTC temperature. Adsorption capacities varied between 9.0 and 68 mg g-1 char, being highest for biosludge treated at 220℃. Adsorption dropped drastically at the highest HTC temperature (260℃), which may be due to the decrease in oxygen-containing functionalities. Also substantial differences were seen between different feedstock materials. 

    Conclusions: These results suggest that adsorption properties can be tailored both by selection of HTC temperature and feedstock.

  • 10.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boily, Jean-Francois
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Bergknut, Magnus
    MTC-Miljötekniskt Center AB, Umeå, Sweden.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    The impact of hydrothermal carbonization on the surface functionalities of wet waste materials for water treatment applications2020In: Environmental Science and Pollution Research, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 27, no 19, p. 24369-24379Article in journal (Refereed)
    Abstract [en]

    Hydrothermal carbonization (HTC) is an energy-efficient thermochemical process for converting wet waste products into value added materials for water treatment. Understanding how HTC influences the physicochemical properties of the resultant materials is critical in optimizing the process for water treatment, where surface functionality and surface area play a major role. In this study, we have examined the HTC of four wet waste streams, sewage sludge, biosludge, fiber sludge, and horse manure at three different temperatures (180 degrees C, 220 degrees C, and 260 degrees C). The physicochemical properties of these materials were examined via FTIR, SEM and BET with their adsorption capacity were assessed using methylene blue. The yield of solid material after hydrothermal carbonization (hydrochar) decreased with increasing temperature for all samples, with the largest impact on horse manure and fiber sludge. These materials also lost the highest degree of oxygen, while HTC had minimal impact on biosludge and sewage sludge. The differences here were due to the varying compositions of each waste material, FTIR identified resonances related to cellulose in horse manure and fiber sludge, which were not detected in biosludge and sewage sludge. Adsorption capacities varied between 9.0 and 68 mg g(-1) with biosludge HTC at 220 degrees C adsorbing the highest amount. Adsorption also dropped drastically at the highest temperature (260 degrees C), indicating a correlation between adsorption capacity and HTC conditions. This was attributed to the loss of oxygen functional groups, which can contribute to adsorption. These results suggest that adsorption properties can be tailored both by selection of HTC temperature and feedstock.

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  • 11.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    From waste to water treatment: Physicochemical and wastewater adsorption properties of activated hydrothermally carbonized waste materialsManuscript (preprint) (Other academic)
    Abstract [en]

    Activated carbon forms an important step in the treatment of waste water in water treatment facilities. These facilities produce a range of underutilized sludge materials, which can be synthesized into activated carbon, reducing the amount of disposed sludge. Other waste materials high in organic matter, such as horse manure, are also ideal contenders for activated carbon upgrading. This study compares the hydrothermal carbonization followed by activation of sewage sludge and horse manure. Chemical activation was conducted using KOH and H3PO4, with physicochemical properties and adsorption of multiple contaminants being tested. Yield and inorganic content varied considerably, with KOH activated materials producing lower yields with higher inorganic content. A maximum surface area of 1363 m2g-1 and 343 m2g-1 was achieved for the horse manure and sewage sludge, respectively. Horse manure activated carbons displayed a high affinity for all adsorbates, other than arsenic, which was associated with high carbon content, carbon-oxygen functional groups and low mineral content.

  • 12.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Industrial Doctoral School, Umeå University.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    The influence of inorganic components and carbon-oxygen surface functionalities in activated hydrothermally carbonized waste materials for water treatment2020In: Environmental Science and Pollution Research, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 27, no 30, p. 38072-38083Article in journal (Refereed)
    Abstract [en]

    In this study, we have examined how the activation of hydrothermally carbonized sewage sludge and horse manure influences the inorganic component of these materials and surface chemistry. This was examined through statistical correlations between kinetic tests using trimethoprim, fluconazole, perfluorooctanoic acid, and copper, zinc, and arsenic and physicochemical properties. Yield and inorganic content varied considerably, with potassium hydroxide-activated materials producing lower yields with higher inorganic content. Phosphoric acid activation incorporated inorganically bound phosphorus into the material, although this showed no statistically relevant benefit. A maximum surface area of 1363 m(2)g(-1)and 343 m(2)g(-1)was achieved for the horse manure and sewage sludge. Statistical analysis found positive correlations between carbon-oxygen functionalities and trimethoprim, fluconazole, perfluorooctanoic acid, and copper removal, while inorganic content was negatively correlated. Conversely, arsenic removal was positively correlated with inorganic content. This research provides insight into the interactions with the organic/inorganic fraction of activated waste materials for water treatment.

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