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Determination of aliphatic and phenolic hydroxyl groups in lignin by chemometric analysis of FTIR spectroscopic data, TAPPI Journal October 2025
Application: Rapid determination of aliphatic and phenolic hydroxyl groups in lignin was achieved using FTIR spectroscopy and chemometric modeling (PCR and PLSR). The PLSR model, particularly when applied to MSCpretreated data, provided accurate predictions for various hydroxyl types (R2 > 0.93), closely aligning with NMRderived values.
Journal articles
Assessing lignin content in Nordic hardwood and softwood species using models based on near-infrared (NIR) spectral data and partial least squares regression (PLSR), TAPPI Journal September 2025
ABSTRACT: Continuous kraft cooking digesters face challenges affecting product quality, making it valuable to improve control through advanced techniques like near-infrared (NIR) spectroscopy, model predictive control, and machine learning models. The primary goal of this study was to use NIR spectra to predict the amount of lignin in hardwood and softwood samples. This study investigated the correlation of NIR derivative spectra with the amounts of lignin relative to other constituents, namely cellulose, hemicellulose, and water, in wood chip samples of varying chip sizes and shapes from six Nordic wood species. It employed partial least squares regression (PLSR) on the NIR data to construct a model that predicted the lignin fraction and the relative fraction of acid-soluble lignin. When trained on a group of five wood species, the model achieved a satisfactory predictive ability, striking a balance between a wide range of lignin content and a consistent chemical environment. The accuracy increased further when the model was restricted only to spruce and pine, reflecting the benefits of a more homogenous dataset. Additionally, the optimal number of latent variables was identified as two, indicating that three distinct chemical components — cellulose, lignin and water — can be effectively differentiated using NIR.
Journal articles
Local delamination in pharmaceutical blister packages • A thermomechanical theory on buckling of heat-sealed composite laminates in flexible packaging, TAPPI Journal July 2025
ABSTRACT: Pharmaceutical blister packages consist of cavities made from a thick polymeric form foil and a thin aluminum lid foil. Heat-sealing technology is usually used to bond the lid foil to the form foil. Occasionally, the sealed area shows buckling defects of the lid foil, which allow contamination to enter into the cavity. A contaminated product is a worst-case scenario for pharmaceutical production and must be avoided. We discuss a thermomechanical theory on buckling defects in blister packages and derive strategies to avoid these. The theory is based on the assumption that the seal of a blister packaging behaves like a laminate of thin composite layers under compressive load. Literature research on buckling of thin laminated films, thermal behavior of polymers, and seal strength of heat-sealed polymers provides the technical and physical background to elaborate the theory. The theory comprises three elements: an initial condition regarding thermal load and precedent defects; a buckling condition; and a crack propagation condition. The plausibility of the theory is verified using model calculations and heat-seal tests. The paper concludes with strategies against buckling of heat-sealed lid foils and an outlook on other applications in laminating and coating of polymer films.
Journal articles
Data-efficient determination of machine-specific process windows in thermoforming using the example of PCR materials, TAPPI Journal July 2025
ABSTRACT: In an industrial context, process windows for thermoplastics in thermoforming processes are still often determined through time-consuming trial-and-error approaches. This results in increased effort when commissioning new machines, implementing new technologies, or substituting sheet materials. One key reason is the lack of methods that allow for efficient, process-related assessment of material behavior and a quantitative definition of a “target state” of the heated sheet in relation to geometry and process conditions. In this study, we present the In-Situ Thermoforming Characterization (ITC) method as an application-oriented approach that enables format-independent evaluation of material behavior directly within the forming station of a thermoforming system. The method was successfully applied to a material substitution case, replacing conventional virgin polypropylene (PP) with post-consumer recyclate (PCR) — in this case, recycled PP (rPP) — in the production of a defined cup geometry. The results enabled the transfer of existing process knowledge from the virgin material to the recyclate, thereby accelerating material qualification. Based on the collected data, material behavior under process conditions could be mapped within the design space, making it possible to identify machine settings that deliver equivalent forming results in our test setup. Overall, the method shows strong potential for efficient and precise determination of machine-specific process windows.
Journal articles
Materials performance considerations in hydrothermal liquefaction conversion of biomass, TAPPI Journal June 2025
ABSTRACT: Hydrothermal liquefaction (HTL) is a promising thermochemical route developed to convert woody biomass and biowaste to biochemicals and bio-oils. However, the operating conditions are rather harsh to biorefinery structural metallic components. These conditions include alkaline catalysts such as potassium carbonate (K2CO3); hot, pressurized (sub-critical) water reaction; and medium and aggressive anions chlorine (Cl•) and hydrogen sulfide (H•) released from biomass feedstocks. Thus, selection of suitable structural alloys for biorefinery components involves striking a balance between mechanical properties, corrosion resistance, and cost. Alloys currently being considered for this application include ferritic-martensitic steels and austenitic stainless steels. From a corrosion perspective in hot pressurized water, the former typically exhibits higher stress corrosion cracking resistance, whereas the latter exhibits higher corrosion resistance. This study reviews cost-effective corrosion control strategies aimed at increasing the chromium (Cr) content for protective surface oxide formation, as screened by testing in simulated HTL alkaline water, to support materials selection and design. Corrosion control strategies include surface modification (increasing surface Cr content), alloying (increasing bulk Cr content), and stainless-steel type (ferritic vs. austenitic). Of the alloys considered (including those subjected to surface modification), ferritic stainless steels exhibit a promising balance between corrosion and stress corrosion cracking resistance, adding another family of candidate alloys for structural biorefinery component materials selection and design.
Journal articles
Pilot-made, highly extensible paper for dry 3D forming, TAPPI Journal May 2025
Cellulose fiber-based packaging materials must perform well in demanding three dimensional (3D) forming process conditions. On the other hand, the development of manufacturing concepts is required for improved competitiveness of bio-based materials. This study covers some key factors that influence the extensibility of cellulose fiber-based structures and presents a pilot-scale development study of a 3D formable material concept. Bleached softwood kraft (BSK) pulp from a Nordic pulp mill was used in the pilot trials. Cellulose-based webs were formed using water-laid and foam-laid web forming using a pilot paper machine. For the water-laid forming, the BSK pulp was refined by applying a high consistency (HC) phase at over 40% consistency, followed by a low consistency (LC) refining at 4% consistency. The BSK pulp was refined for the foam-laid forming by only applying lowconsistency refining. In the foam-laid web forming, anionic sodium dodecyl sulfate (SDS), two foamable latexes, and polyvinyl alcohol (PVA) were used as foaming agents. The pilot rolls were dried at a separate steam cylinder dryer pilot and compacted in-plane in the machine direction (MD) at a separate pilot machine. Tensile properties of the treated paper webs were measured and evaluated with respect to achieved web shrinkage. The same dimensional contraction brought by shrinkage was almost strained out in tensile testing. The results indicated that the shrinkage that occurred by drying and in-plane compaction depended on the pulp furnish. The water-laid material achieved about 30% elongation, whereas the foam-laid material achieved significantly above 50% elongation. The 3D forming performance of the dry materials was tested using fixed and sliding blank methods. The dry paper sheets performed well enough in 3D forming for application to many consumer package applications according to their extensibility.
Journal articles
Magazine articles
Study on the effect of aluminum diethyl phosphinate in synergy with ammonium polyphosphate on the flame retardancy of cellulose paper, TAPPI Journal April 2025
ABSTRACT: This paper involved the synergistic incorporation of ammonium polyphosphate (APP) and diethyl aluminum phosphinate (AlPi) as flame-retardant fillers for producing flame-retardant paper. The research revealed that APPs were square particles with a smooth surface, and their solubility was 0.29 g/100 mL at 20°C, which increased to 4.12 g/100 mL at 60°C. The surfaces of AlPis were rough and irregular. The solubility of AlPi was 0.023 g/100 mL at 20°C, and the solubility remained stable when the temperature increased. The addition of AlPi had a minor influence on the pulp beating degree. The tensile strength of kraft/APP/AlPi decreased with the increase of the AlPi addition. For a paper with 20 wt% APP and 0 wt% AlPi, the limiting oxygen index (LOI) value was 27.2%, and it burned completely at the eighth second during vertical combustion. When the AlPi additive content increased to 20 wt%, its LOI value increased to 32.2%, and the vertical combustion self-extinguished as soon as the flame was removed. Scanning electron microscopy (SEM) showed that the char residue of the kraft/APP/AlPi had a more complete fiber network structure than that of kraft/APP. The Raman spectroscopy indicated that the area ratio of the D (amorphous phase; disordered graphite vibration) band to the G (crystal phase; graphite carbon vibration) band (ID/ IG) ratio of kraft/APP/AlPi was lower than that of kraft/APP, meaning that the graphitization degree of the char residue of kraft/APP/AlPi was higher than that of kraft/APP, which indicated the kraft/APP/AlPi had better flame retardancy.
Journal articles
Magazine articles
Modeling the dynamics of evaporator wash cycles, TAPPI Journal July 2024
ABSTRACT: Kraft pulping is a process that utilizes white liquor, composed of sodium sulfide (Na2S) and sodium hydroxide (NaOH), for wood delignification and pulp production. This process involves washing the dissolved organics and spent chemicals from the pulp, resulting in the generation of black liquor. Prior to its use as fuel in the recovery boiler, the black liquor is concentrated in multiple-effect evaporators. During the evaporation process, the inorganic salts present in the liquor become supersaturated and undergo crystallization. Fluctuations in sodium, carbonate, sulfate, and oxalate can give rise to severe sodium salt scaling events, which significantly impact the thermal efficiency of the evaporators, and ultimately, pulp production. Dynamic modeling provides insights into fluctuations in liquor chemistry in the evaporators. The primary objective of this study was to employ dynamic modeling to evaluate the effects of wash liquor recovery from evaporator wash cycles. The dynamics associated with wash cycles encompass variations in the concentrations of salts and solids in the recovered wash liquor, changes in the flow rate of wash liquor recovery, and fluctuations in liquor volume within the liquor tanks. The dynamic model was developed using Matlab Simulink and applied to the evaporation plant of a pulp mill in South America. By utilizing one month of mill process data, the model enabled the evaluation of fluctuations in liquor chemistry due to evaporator wash cycles. The developed model has demonstrated the potential to estimate the concentration of key ions responsible for scaling and to contribute to enhancements in evaporator washing strategies.
Journal articles
Magazine articles
Online monitoring of the size distribution of lime nodules in a full-scale operated lime kiln using an in-situ laser triangulation camera, TAPPI Journal June 2024
ABSTRACT: To maximize efficiency of the recausticizing process in a pulp mill, producing a reburned lime with high and consistent reactivity is process critical. Prior investigations have demonstrated a correlation between the reactivity of lime and its nodule size, as well as the dusting behavior of the kiln. Therefore, monitoring the nodule size produced in the lime kiln could be a promising indirect method to measure the performance of the lime kiln. The objective of this investigation was to evaluate the utility of a laser triangulation camera for online monitoring of nodule size distribution for the lime kiln. A series of full-scale trials were performed in a lime kiln of a kraft pulp mill in which a camera was installed at the exit conveyor to analyze the lime discharging from the kiln. The nodule size distribution was analyzed for correlation with the lime temperature, flue gas temperature, and rotational speed of the kiln. The monitoring demonstrated temporal stability, and the results showed that the lime temperature had the most significant effect on the nodule size. The rotational speed of the lime kiln and the flue gas temperature showed limited effect on nodule size, but they had significant impact on the specific energy demand. The overall conclusion of the study is that the camera methodology effectively correlates lime temperature with nodule size distribution, and it advocates for the methods of implementation in automating lime temperature control, facilitating the production of consistently reactive lime at a lower specific energy consumption.
Journal articles
Magazine articles
Understanding the energy and emission implications of new technologies in a kraft mill: Insights from a CADSIM Plus simulation model, TAPPI Journal June 2024
ABSTRACT: Kraft mills play a vital role in energy transition because they have significant potential to reduce their own energy utilization and produce energy/products to decarbonize other sectors. Through biomass combustion and potential biogenic carbon emissions capture, these mills can contribute to offsetting emissions from other sectors. This research investigates the departmental and cross-departmental implications of technology upgrades on energy, steam, emissions, water, and chemicals using a CADSIM Plus simulation model. The model provides a comprehensive analysis of mass and energy balances, offering valuable insights into the benefits and limitations of each technology. The model facilitates scenario analysis and comparisons of process configurations, enabling data-driven decision-making for sustainable and competitive operations. Six high-impact technologies, including additional evaporator effects, weak black liquor membrane concentration, belt displacement washer for brownstock washing, oxygen delignification, and improvements to the pulp machine shoe press and vacuum pumps, are evaluated. Individual technologies resulted in energy savings of 1.2% to 5.4%, biomass consumption reductions of 8.6% to 31.6%, and total emissions reductions of 1.6% to 5.9%. Strategic decision-making must consider existing mill limitations, future technology implementation, and potential production increases. Future research will explore product diversification, biorefineries, and pathways to achieve carbon-negative operations, aiming to reduce emissions and secure a competitive future for kraft mills.