Drying, Grinding and Pelletization Studies on Raw
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09 BIOMASS FUELS↗
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Reactive Grinding of Coal Ash for Enhanced Rare Earth Extraction
Presented by NETL at AICHE National Meeting, 11/16
Roth, Elliot↗
Particle scale impacts on deconstruction energy of pine residues
The goal of this Case Study was to quantify the impacts of variable moisture and ash on hammer mill throughput and energy consumption and on generation of fines that are not able to be fed to conversion, as compared to a status quo Base Case system. Also considered was convertible carbon content (minimum carbon specification) and maximum ash content and the delivered feedstock cost impacts of not being able to feed residue not meeting both specifications to the conversion reactor. Laboratory data on the impacts of input particle size and moisture content on the exit particle size were received from FCIC Subtask 5.2 from their single particle impact population balance modeling study. Additional throughput and energy consumption data were obtained from FCIC Subtask 5.2 for the same grinder with a 6 mm screen in place. These data were utilized to develop the necessary response surface equations to perform throughput analysis using discrete event simulation. Because the ash contents in the separated fines had not been analyzed in the laboratory at the time of the model runs, we chose to assume that the ash distributed proportionally with total mass into the overs and unders in the disk screen following grinding. Key takeaways from this Case Study are that it is significantly more cost effective to hammer mill the residue prior to drying, even though the grinder throughput is lower and energy consumption is higher versus drying first before grinding. An effect of dry grinding versus high moisture grinding is the production of higher amounts of fines during dry grinding, leading to significantly more of the ground feedstock being rejected by conversion for being below a minimum particle size. With wet grinding the system is still able to produce more preprocessed feedstock meeting the minimum particle size specification even though the instantaneous throughput is lower than for the case of grinding dry feedstock. Additionally, even without the higher fines production from dry grinding, the status quo would still be more costly than wet grinding because the material is rejected after the drying energy has already been input for the dry grinding case. Finally, significant reductions in drying energy are obtained by drying after grinding, and those reductions are of far greater magnitude than the grinding energy increase.
09 BIOMASS FUELS↗
Nitrogen-doped graphene catalysts: High energy wet ball milling synthesis and characterizations of functional groups and particle size variation with time and speed
Nitrogen-doped graphene (N-G) catalyst emerges as one of the promising non-platinum group metal (non-PGM) catalysts with the advantages of low cost, high oxygen reduction reaction (ORR) activity, stability, and selectivity to replace expensive PGM catalysts in electrochemical systems. This research investigated nanoscale high energy wet (NHEW) ball milling for the synthesis of N-G catalysts to make conventional problems such as sintering or localized overheating issues negligible. The successful synthesis of N-G catalysts with comparable catalytic performance to 10 wt% Pt/C by using this method has been published. This paper focuses on understanding the effect of grinding speed and grinding time on the particle size and chemical state of N-G catalysts through the physical and chemical characterization. The research result shows that (1) the final particle size, nitrogen doping percentage, and nitrogen bonding composition of synthesized N-G catalysts are predictable and controllable by adjusting the grinding time, the grinding speed, and other relative experimental parameters; (2) the final particle size of N-G catalysts could be estimated from the derived relation between the cracking energy density and the particle size of ground material in the NHEW ball milling process with specified experimental parameters; and (3) the chemical composition of N-G catalysts synthesized by NHEW ball milling is controllable by adjusting the grinding time and grinding speed.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Enhanced grindability of bastnaesite ore by ex-situ CO 2 treatment under the partial pressure of 0-100 psi
High grinding energy consumption has long constrained the sustainable development of mineral processing. This study introduces an innovative technology that employs ex-situ CO 2 treatment to enhance the grindability of bastnaesite ore. The grinding aid effect was evaluated under CO 2 partial pressures ranging from 0 psi to 100 psi using particle size distribution and the Bond work index (BWI), while the underlying mechanism was elucidated with various characterization techniques including inductively coupled plasma (ICP), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and Brunauer-Emmett-Teller (BET). The optimal grinding aid effect was achieved at 100 psi partial pressure, 50% slurry concentration, and 3 h reaction duration. Correspondingly, the P80 of the grinding product decreased from 81.76 μm to 72.73 μm and the BWI of bastnaesite ore decreased from 6.96 kW·h/t to 6.30 kW·h/t, a reduction of 9.48%. The grinding aid effect primarily resulted from the transformation of sparingly soluble carbonates like calcite and dolomite into more soluble bicarbonates, which created substantial cracks and pores, thereby reducing the ore's hardness and improving its grindability. By significantly saving grinding energy consumption while delivering environmental benefits, this technology exhibits great promise for further optimization and widespread adoption.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides
A mechanochemical method (grinding the components without added water – dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution – wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic–inorganic nanocomposites: LDHs intercalated with amino acid anions. - Graphical abstract: Amino acid anion-Ca(II)Fe(III)-LDHs were successfully prepared by a two-step milling procedure. - Highlights: • Synthesis of pristine and amino acid intercalated CaFe-LDHs by two-step milling. • Identifying the optimum synthesis and intercalation parameters. • Characterisation of the samples with a range of instrumental methods.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Effect of solvent fractionation pretreatment on energy consumption of cellulose nanofabrication from switchgrass
Lignin-containing cellulose nanofibers (L-CNFs) with various lignin contents were produced by a grinding process from switchgrass, which were pretreated using organosolv fractionation. The effect of different fractionation conditions (temperature and time) and different number of grinder passes on the energy consumption and morphologies of L-CNFs were investigated. Results revealed that nanosized fibers were found in organosolv-fractionated samples before grinding. After several grinding passes, L-CNFs with a similar degree of fibrillation as commercial cellulose nanofibers (CNF) were obtained from the fractionated materials. It is beneficial to save energy consumption in the grinding process. The dimensions and dispersion of L-CNFs were significantly influenced by the lignin content in the L-CNFs. Longer and well-separated nanofibrils were observed from transmission electron microscopy and fluorescence microscopy with appropriate residual lignin (~ 13.7 ± 1.59%) in the L-CNFs compared to those of L-CNFs with either lower or higher lignin contents. Thus, microsized and nanosized lignin particles were successfully obtained in a single process, and they not only facilitated L-CNFs dispersion but also help to decrease the energy consumption during the grinding process.
09 BIOMASS FUELS↗
Permissible Exposure Level for Lunar Dusts: Gaps are Closing
Space faring nations plan to return human explorers to the moon within the next decade. Experience during the Apollo flights suggests that lunar dust will invariably get into the habitat where the finest portion (less than 5 micrometers) could be inhaled by the crew before it is cleared from the atmosphere. NASA is developing a database from which a 6-month, episodic exposure standard for lunar dust can be set. Three kinds of moon dust were prepared from a parent sample of Apollo 14 regolith #14003,96. Our goal was to prepare each type of dust sample with a mean diameter less than 2 m, which is suitable for instillation into the lungs of rats. The three samples were prepared as follows: separation from the parent sample using a fluidized bed, grinding using a jet mill grinder, or grinding with a ball-mill grinder. Grinding simulated restoration of surface activation of dust expected to occur at the surface of the moon on native lunar dust. We used two grinding methods because they seemed to produce different modes of activation. The effects of grinding were preserved by maintaining the dust in ultra-pure nitrogen until immediately before it was placed in suspension for administration to rats. The dust was suspended in physiological saline with 10% Survanta, a lung surfactant. Rats were given intratrachael instillations of the dust suspension at three doses. In addition to the three moon dusts (A, C and E), we instilled the same amount of a negative control (TiO2, B) and a highly-toxic, positive control (quartz, D). These additional mineral dusts were selected because they have well-established and very different permissible exposure levels (PELs). Our goal was to determine where lunar dusts fit between these extremes, and then estimate a PEL for each lunar dust. We evaluated many indices of toxicity to the lung. The figure shows the changes in lactate dehydrogenase (LDH), a marker of cell death, for the five dusts. Benchmark dose software (Version 2.1.2) from the Environmental Protection Agency was used to estimate the 10% effect levels (BMD(sub 10)) using five models. The best-fitting model was used to estimate the optimal BMD(sub 10) (table)
James, John T.↗
Semiautomated, Reproducible Batch Processing of Soy
A computer-controlled apparatus processes batches of soybeans into one or more of a variety of food products, under conditions that can be chosen by the user and reproduced from batch to batch. Examples of products include soy milk, tofu, okara (an insoluble protein and fiber byproduct of soy milk), and whey. Most processing steps take place without intervention by the user. This apparatus was developed for use in research on processing of soy. It is also a prototype of other soy-processing apparatuses for research, industrial, and home use. Prior soy-processing equipment includes household devices that automatically produce soy milk but do not automatically produce tofu. The designs of prior soy-processing equipment require users to manually transfer intermediate solid soy products and to press them manually and, hence, under conditions that are not consistent from batch to batch. Prior designs do not afford choices of processing conditions: Users cannot use previously developed soy-processing equipment to investigate the effects of variations of techniques used to produce soy milk (e.g., cold grinding, hot grinding, and pre-cook blanching) and of such process parameters as cooking times and temperatures, grinding times, soaking times and temperatures, rinsing conditions, and sizes of particles generated by grinding. In contrast, the present apparatus is amenable to such investigations. The apparatus (see figure) includes a processing tank and a jacketed holding or coagulation tank. The processing tank can be capped by either of two different heads and can contain either of two different insertable mesh baskets. The first head includes a grinding blade and heating elements. The second head includes an automated press piston. One mesh basket, designated the okara basket, has oblong holes with a size equivalent to about 40 mesh [40 openings per inch (.16 openings per centimeter)]. The second mesh basket, designated the tofu basket, has holes of 70 mesh [70 openings per inch (.28 openings per centimeter)] and is used in conjunction with the press-piston head. Supporting equipment includes a soy-milk heat exchanger for maintaining selected coagulation temperatures, a filter system for separating okara from other particulate matter and from soy milk, two pumps, and various thermocouples, flowmeters, level indicators, pressure sensors, valves, tubes, and sample ports
Thoerne, Mary↗
Hydriding and dehydriding characteristics of LiBH{sub 4} and transition metals-added magnesium hydride
Graphical abstract: Hydriding reaction curves under 12 bar H{sub 2}, and dehydriding reaction curves under 1.0 bar H{sub 2}, at 593 K at the 1st cycle for MgH{sub 2}–10Ni–2LiBH{sub 4}–2Ti and MgH{sub 2}. Highlights: ► Addition of Ni, LiBH{sub 4}, and Ti to MgH{sub 2} to increase reaction rates. ► Sample preparation by reactive mechanical grinding. ► At n = 2, the sample absorbed 4.05 wt% H for 60 min at 593 K under 12 bar H{sub 2}. ► Analysis of rate-controlling step for dehydriding of the sample at n = 3. - Abstract: In this study, MgH{sub 2} was used as a starting material instead of Mg. Ni, Ti, and LiBH{sub 4} with a high hydrogen-storage capacity of 18.4 wt% were added. A sample with a composition of MgH{sub 2}–10Ni–2LiBH{sub 4}–2Ti was prepared by reactive mechanical grinding. The activation of MgH{sub 2}–10Ni–2LiBH{sub 4}–2Ti was completed after the first hydriding–dehydrding cycle. The hydriding rate decreases as the temperature increases due to the decrease in the driving force for the hydriding reaction. At the 1st cycle, the sample desorbs 1.45 wt% H for 10 min, 2.54 wt% H for 20 min, 3.13 wt% H for 30 min, and 3.40 wt% H for 60 min at 593 K under 1.0 bar H{sub 2}. At the 2nd cycle, the sample absorbs 3.84 wt% H for 5 min, 3.96 wt% H for 10 min, and 4.05 wt% H for 60 min at 593 K under 12 bar H{sub 2}. MgH{sub 2}–10Ni–2LiBH{sub 4}–2Ti after reactive mechanical grinding contained MgH{sub 2}, Mg, Ni, TiH{sub 1.924}, and MgO phases. The reactive mechanical grinding of Mg with Ni, LiBH{sub 4}, and Ti is considered to create defects on the surface and in the interior of Mg (to facilitate nucleation), and to reduce the particle size of Mg (to shorten diffusion distances of hydrogen atoms). The formation of Mg{sub 2}Ni during hydriding–dehydriding cycling increases the hydriding and dehydriding rates of the sample.
36 MATERIALS SCIENCE↗
Enzymantic Conversion of Coal to Liquid Fuels
The work in this project focused on the conversion of bituminous coal to liquid hydrocarbons. The major steps in this process include mechanical pretreatment, chemical pretreatment, and finally solubilization and conversion of coal to liquid hydrocarbons. Two different types of mechanical pretreatment were considered for the process: hammer mill grinding and jet mill grinding. After research and experimentation, it was decided to use jet mill grinding, which allows for coal to be ground down to particle sizes of 5 {mu}m or less. A Fluid Energy Model 0101 JET-O-MIZER-630 size reduction mill was purchased for this purpose. This machine was completed and final testing was performed on the machine at the Fluid Energy facilities in Telford, PA. The test results from the machine show that it can indeed perform to the required specifications and is able to grind coal down to a mean particle size that is ideal for experimentation. Solubilization and conversion experiments were performed on various pretreated coal samples using 3 different approaches: (1) enzymatic - using extracellular Laccase and Manganese Peroxidase (MnP), (2) chemical - using Ammonium Tartrate and Manganese Peroxidase, and (3) enzymatic - using the live organisms Phanerochaete chrysosporium. Spectral analysis was used to determine how effective each of these methods were in decomposing bituminous coal. After analysis of the results and other considerations, such as cost and environmental impacts, it was determined that the enzymatic approaches, as opposed to the chemical approaches using chelators, were more effective in decomposing coal. The results from the laccase/MnP experiments and Phanerochaete chrysosporium experiments are presented and compared in this final report. Spectra from both enzymatic methods show absorption peaks in the 240nm to 300nm region. These peaks correspond to aromatic intermediates formed when breaking down the coal structure. The peaks then decrease in absorbance over time, corresponding to the consumption of aromatic intermediates as they undergo ring cleavage. The results show that this process happens within 1 hour when using extracellular enzymes, but takes several days when using live organisms. In addition, live organisms require specific culture conditions, control of contaminants and fungicides in order to effectively produce extracellular enzymes that degrade coal. Therefore, when comparing the two enzymatic methods, results show that the process of using extracellular lignin degrading enzymes, such as laccase and manganese peroxidase, appears to be a more efficient method of decomposing bituminous coal.
01 COAL, LIGNITE, AND PEAT↗
Charged Porous Polymers using a Solid C-O Cross-Coupling Reaction
We report a green, fast, efficient mechanochemical strategy for charged porous polymers (CPPs). A cationic CPP with basic anions and an anionic CPP with Li + cations were fabricated by solid grinding under solvent- free conditions. Compared with solution-based synthesis, mechanochemical grinding can shorten the reaction time from dozens of hours to several minutes (60– 90 min) to form polymers possessing a high molecular mass and low polydispersity. During the construction of CPPs, a Pd-catalyzed solid polycondensation based on unactivated organic linkers was introduced. In particular, CPPs with basic phenolic or proline anions showed good activity and stability in SO 2 capture, and Li + -functionalized CPPs can be post-modified to CPPs with other metal ions by ion exchange, highlighting the tailorable feature of ionic-modified CPPs.
36 MATERIALS SCIENCE↗
Assessment of the grindability of robocast silicon carbide
The demand for high-performance lightweight optics has driven interest in silicon carbide (SiC) due to its exceptional thermal stability, hardness, and strength-to-weight ratio. This study investigates the potential of robocasting, an additive manufacturing process, as a viable method for producing lightweighted SiC components for optical applications. Four samples with varied starting powder phases (α and β) and sintering conditions were fabricated and evaluated. Post-sintering surface and form were assessed using coherence scanning interferometry (CSI) and coordinate measuring machine (CMM) techniques. A three-stage grinding process was applied to each sample, with surface roughness assessed at each stage. Results demonstrate that samples with predominantly α-phase SiC and smaller particle sizes achieved superior surface finish, particularly sample D2-α-2135 °C, which displayed the lowest post-grinding Sq value of 0.178 µm. The analysis also indicated no significant print-through effect from the lightweighting structure, or print artifacts, at this stage of grinding. However, β-phase samples showed poorer grindability, increased surface roughness, and pitting. These findings suggest that phase composition and particle size are critical for achieving the desired surface quality in robocast SiC optics. Future work will incorporate additional samples and finer grinding wheels to refine surface quality further, supporting the development of SiC for high-precision optical applications.
Barrett, Taylor [ORNL]↗
Liberation and release of rare earth minerals from Middle Kittanning, Fire Clay, and West Kentucky No. 13 coal sources
Here, a laboratory REE release test procedure was designed to better understand the association and liberation characteristics of rare earth elements (REEs) from coal-based material, such as coal middlings and refuse. For this particular study, three samples of mixed-phase, middling material was collected from three coal preparation plants operating in three different coal basins and coal seams, namely Fire Clay, Middle Kittanning, and West Kentucky #13. In these release tests, the mixed-phase material was first ground in a laboratory ball mill for a designated amount of time and subsequently decarbonized using staged flotation. The REE content of the high ash tailings and low ash concentrate was determined, and the process was repeated for various target grind sizes down to the micron range. The results indicate that smaller grind sizes produce increased REE concentrations in the high ash tailings, and this result is predominantly driven by the increased ash content in the decarbonized tailings. The grinding characteristics of the Fire Clay coal source showed that more energy is needed to achieve the desired particle size reduction; however further size reduction of this sample resulted in a significantly higher ash and REE content in the tailings material due to improved liberation. For the Middle Kittanning and West Kentucky #13 sources, the grinding and release data indicates that the mineral matter is liberated at a coarser particle size, and micronizing the coals only produces marginal improvements in rare earth mineral liberation and recovery.
01 COAL, LIGNITE, AND PEAT↗
Intelligent Manufacturing of Commercial Optics Final Report CRADA No. TC-0313-92
The project combined the research and development efforts of LLNL and the University of Rochester Center for Manufacturing Optics (COM), to develop a new generation of flexible computer controlled optics· grinding machines. COM's principal near term development effort is to commercialize the OPTICAM-SM, a new prototype spherical grinding machine. A crucial requirement for commercializing the OPTICAM-SM is the development of a predictable and repeatable material removal process ( deterministic micro-grinding) that yields high quality surfaces that minimize non-deterministic polishing. OPTICAM machine tools and the fabrication process development studies are part of COM' s response to the DOD (ARPA) request to implement a modernization strategy for revitalizing the U.S. optics manufacturing base. This project was entered into in order to develop a new generation of :flexible, computer-controlled optics grinding machines.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Spherical artifacts on ferrograms
In the past, hollow spheres detected on ferrograms have been interpreted as being due to fretting, abrasion, cavitation erosion, and fatigue-related processes. Here it is reported that such spheres were found to result from the fact that a routine grinding operation on a steel plate was carried out about 20 feet away from the ferrograph. A similar grinding operation was performed on a piece of low carbon steel a few feet from the ferrograph, and after a few minutes of grinding, the resulting ferrogram contained thousands of particles of which more than 90% were spherical. Because of the widespread occurrence of ordinary grinding operations, it seems prudent that those utilizing the ferrograph be cognizant of this type of artifact.
Jones, W. R., Jr.↗
Milling and mechanical alloying of inorganic nonmetallics
The versatility of high energy grinding for instigating mechanochemical reactions in inorganic systems has been studied. High-energy grinding can be used to produce amorphous carbon from synthetic graphite and some forms of natural graphite. Elemental sulfur can be amorphized by prolonged energy grinding. The presence of iron resulting from wear of the grinding media strongly affects phase transformations of alphaFe2O3 and mechanochemical reactions of this phase with ZnO and NiO. Data obtained confirm that low-temperature mechanochemical method is a robust process route for production of a wide range of materials.
Kosmac, T.↗
Dynamic Fatigue of ULE Glass
Ultra Low Expansion (ULE) glass is used in a number of applications which require a low thermal expansion coefficient. One such application is telescope mirror elements. An allowable stress can be calculated for this material based upon modulus of rupture data; however, this does not take into account the problem of delayed failure. Delayed failure, due to stress corrosion can significantly shorten the lifetime of a glass article. Knowledge of the factors governing the rate of subcritical flaw growth in a given environment enables the development of relations between lifetime, applied stress and failure probability for the material under study. Dynamic fatigue is one method of obtaining the necessary information to develop these relationships. In this study, the dynamic fatigue method was used to construct time-to-failure diagrams for both 230/270 ground and optically polished samples. The grinding and polishing process reduces the surface flaw size and subsurface damage, and relieves residual stress by removing materials with successively smaller grinding media. This resulted in an increase in the strength of the optic during the grinding and polishing sequence. There was also an increase in the lifetime due to grinding and polishing. It was found that using the fatigue parameters determined from the 230/270 grit surface are not significantly different from the optically polished values. Although the lower bound of the polished samples is more conservative, neither time-to-failure curves lie beyond the upper or lower bound of the confidence limits. Therefore, designers preferring conservative limits could use samples without residual stress present (polished samples) to determine the fatigue parameters and inert Weibull parameters from samples with the service condition surface, to determine time-to-failure of the optical element.
Tucker, Dennis S.↗