Wet Ball Milling Research Articles

Formulation and optimization of transferrin-modified genistein nanocrystals: In vitro anti-cancer assessment and pharmacokinetic evaluation

In this research work, nanocrystals (NC) of poorly water-soluble drug genistein (Gen) were formulated to improve its aqueous solubility and bioavailability. Genistein nanocrystals (Gen–NC) were prepared by wet ball milling. The formulation was optimized using Box Behnken Design Expert to evaluate the impact of stabilizer concentration, drug concentration and quantity of zirconium beads (milling media) on NC size, polydispersity and zeta potential. The NCs were surface-decorated with transferrin (Tf) to form Tf modified Gen-NCs (Tf-Gen-NC) for improving cancer cell selectivity and cytotoxicity. The NC formulations were characterized by dynamic light scattering (DLS), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, X-ray power diffraction (XRD) and differential scanning calorimetry (DSC). The particle size distribution of the optimized formulation varied from 200 to 300 nm with poly dispersibility index (PDI) between 0.1 and 0.3. Tf-Gen-NC and Gen-NC released 96 % and 80 % of the drug content in 20 min at 37 °C, respectively, whereas only 18 % were released with the unprocessed drug. In vitro cytotoxicity was tested in pulmonary adenocarcinoma epithelial cells (A549) and fibroblast cell line (L929). The Tf-Gen-NC presented an enhanced anticancer effect. In vivo pharmacokinetic studies in mice after intraperitoneal administration showed that the Cmax of NC formulations were 2.5-fold higher compared to free Gen. The area under the curve from time of administration to 24 h was 2.5 to 3-fold higher when compared with unprocessed drug. This study shows the interest of Gen-NC in the development of new formulations for Gen as an anticancer drug.

Effects of synergistic application of Viscozyme L–wet ball milling on structural, physicochemical and functional properties of insoluble dietary fiber from ginseng residue

Synergistic effect of Viscozyme L with wet ball milling treatment on structural, physicochemical and functional aspects of insoluble dietary fiber (IDF) from ginseng residue were examined. SEM examination showed that IDF extracted by Viscozyme L in conjunction with wet ball milling (WBE-IDF) exhibited loose microstructural arrangement, and particle size of WBE-IDF was much smaller than that of IDF extracted by Viscozyme L (E-IDF) and along IDF (untreated). The FTIR spectra demonstrated the variations in the peak intensities in three modified ginseng IDFs. Besides, the highest thermal stability and viscosity was displayed by WBE-IDF among examined samples. In addition, WBE-IDF has higher water and oil holding, water swelling, nitrite ion absorption, bile acid absorption, and glucose absorption capacities as compared to that of E-IDF and IDF. Overall results revealed that the Viscozyme L combined with wet ball milling extraction may change ginseng IDF structure, and improve its physicochemical and functional qualities, thereby providing a theoretical basis for food industry to produce good ginseng IDF.

Wet ball milling activated oyster shells for multifunctional slow-release compound fertilizer production

Slow-release fertilizers have been known to boost crop yields, but their high cost and slow degradation make them less practical for use. In this study, oyster shell (OS) was modified by mechanical ball milling with monosodium glutamate (MSG) wastewater as an activator to prepare activated oyster shell (AOS) with an average particle size of 32.7 nm. Compared to natural oyster shell (NOS), the AOS increased water-soluble Ca by 22 times, expanded the average desorption pore size by 155 %, enhanced the specific surface area by 9 times, and improved the total pore volume by 1587 %. AOS was mixed with traditional fertilizers and extruded to develop a new type of activated oyster-based slow-release compound fertilizer (AOF). Physical effects mainly controlled the slow-release ability of AOF. AOS formed vaterite with a large peak shape, high strength, and well-defined crystal structure, providing more binding sites for NH4+, HPO42−, K+, Ca2+ and Mg2+. In addition, AOS was rich in Ca-OH and Mg-OH, which increased the potential for ligand exchange with fertilizer ions, which further improved the chemical slow-release properties of AOF. The AOF continuously releases N, P, K, Ca, and Mg nutrients over a period exceeding 70 days. The nutrient release behavior in AOF was accurately described by the logistic equation, the Elovich equation, and the parabolic diffusion equation. AOF increased the dry weight of green plum by 190 % and the yield by 61 %. The AOF prepared in this study proved to be an innovative and environmentally sustainable slow-release fertilizer.

Fly ash-based zeolite/reduced graphene oxide/polymer anti-corrosion coatings for efficient heat dissipation

Industries are demanding more and more for the high corrosion protection and thermal conductivity of organic coatings. However, organic coatings always have low thermal conductivity, and the effective distribution of inorganic particles within these organic coatings remains imperative for further enhancing both anti-corrosion and thermal conductivity capabilities simultaneously. Herein, a novel method is introduced for the exfoliation of reduced graphene oxide (rGO) through wet ball milling, incorporating fly ash-based zeolites. The resulting particles (A-rGO) formed two structures: rGO sheets wrapped around or partially loaded on the surface of zeolite particles. Notably, the absolute zeta potential of A-rGO measures 47.8, marking a 4.26-fold increase compared to rGO, thereby facilitating enhanced dispersion within the coating matrix. Then, benzoxazine/A-rGO based coatings are made, which formed a thermally conductive pathway and constructed an anti-corrosion barrier. The results showed that the highest thermal conductivity of the prepared coating (A-r-2) was as high as 1.561 W·m−1 K−1, which was 676.1 % higher than that of benzoxazine based coating, and 159.7 % higher than that of the same content of benzoxazine/rGO coating. Furthermore, the low-frequency impedance value of the A-r-2 coating reached 2.433 × 109 Ω·cm2 with a water contact angle as high as 129.8 ± 0.2°. The particles designed in this study provides a new system additive for fabricating highly thermally conductive composite coatings with high corrosion resistance.

Investigation of the Chemical Changes from N-Doped Graphene and MOF to N-G/MOF Composites for the Enhancement of Electrocatalytic Properties

N-doped graphene (N-G) materials showed high potential as electrocatalysts for oxygen reduction reaction (ORR) in electrochemical energy systems and increasingly gaining ground as alternatives to the expensive and degradation-prone Platinum Group Metal (PGM)-based electrocatalysts. Numerous studies demonstrated that as N-G materials are integrated with Metal-Organic Frameworks (MOFs), the N-G/MOF composites exhibited higher electrocatalytic activities than the individual precursors; on several occasions, even higher than the PGM-based ones. In this essence, it is crucial to analyze and understand the chemical changes that occur through the integration of N-G and MOF, as these changes play key roles in enhancing electrocatalytic properties of the materials by introducing different electrochemically active sites. To investigate such chemical changes, we have synthesized an N-G/MOF composite by integrating an N-G with ZIF-8 (which is the most studied member of the MOF family) following a facile mechanochemical wet ball milling process. In the electrochemical characterization, the N-G/MOF composite performed better than N-G and ZIF-8 for ORR catalysis by generating a higher cathodic current density.Multiple samples of N-G, ZIF-8, and N-G/MOF composite were analyzed by X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy to detect the changes in elemental ratios, chemical bonds, and chemical functional groups from the precursors (N-G and ZIF-8) to the N-G/MOF composite. An increase in the elemental Nitrogen (N) ratio was observed in N-G/MOF compared to its precursors; which signifies an increased N-doping ratio in the material which is advantageous for ORR catalysis. The XPS C 1s spectra of N-G/MOF shifted to a higher binding energy (~1eV) compared to the precursors indicating an overall increase in the oxidation states of Carbon (C) atoms in the material which could facilitate oxygen molecules’ adsorption better on these sites at the beginning of ORR process. Comparing the analyzed XPS N 1s spectra revealed an increased relative ratio of the Pyridinic-N functional group in N-G/MOF, which also partly justifies the composite’s enhanced ORR electrocatalytic performance. FTIR analysis revealed interactions between methyl groups (-CH3) of ZIF-8 with oxygen functional groups (i.e. -OH) of N-G while forming the N-G/MOF composite. Besides, a transition from methyl groups (-CH3) to methylene group ( >CH2) was evident during the synthesis, increasing charge density near those C atoms of the N-G/MOF which can as well be advantageous for ORR electrocatalysis. The combined impact of these chemical alterations from N-G and ZIF-8 to N-G/MOF yielded a synergistic effect, elucidating its superior electrocatalytic properties. The findings of this experimental investigation provide insights into the chemical reasons for the enhancement of electrocatalytic properties of N-G/MOF composites; and hereby offer guidance to the design and optimization endeavors of novel catalysts with N-G and MOF materials for diverse electrochemical applications.

Cellulose binary coatings with spherical envelope structure via structure rearrangement in ball milling for integrated radiative cooling-electricity generation

Passive daytime radiative cooling is a zero-energy consumption cooling technology, which can dissipate heat to outer space via infrared radiation. Recently, coupling radiative cooling technology and thermoelectric devices to generate electricity has attracted much attention. However, existing radiative cooling integrated thermoelectric devices still suffer from low-temperature gradient and output voltage. Here, based on the Mie scattering and internal reflection enhancing principle, an impact-inducing geometry reconstruction approach was proposed to fabricate hierarchical nanostructured cellulosic coatings with good daytime cooling performance to achieve stable electricity generation function, which can be realized by using a scalable and facile wet ball milling technology. Guided by the theoretical simulations of the finite difference time domain method (FDTD), the cellulose and TiO2 nanoparticles can assemble into spherical envelope structured coatings drying by the shear, impact, and friction interaction in the ball milling process, dramatically enhancing the Mie scattering and internal reflection of coatings. The cellulosic coatings exhibit sunlight reflectivity of 0.962 and infrared emissivity of 0.94, resulting in a daytime radiative cooling efficiency of 5.9 °C under direct sunlight. Energy Plus stimulation demonstrated 35 % cooling energy and 468.9 kWh of cooling energy can be saved annually in China. Meanwhile, this cellulosic coating-based thermoelectric device can deliver a high voltage output of 150 mV under 1 Sun due to the strong bonding and high-temperature gradient formation (30 °C), which is higher than previous reports. This study will facilitate the development of sustainable power generation device for the goal of green future.

Improving interfacial magnetoelastic effect and complex permeability of FeSiAl alloy powders for broadband decimeter-wave absorption via Cr doping

This study showcases the interfacial magnetoelastic effect observed in flaky FeSiAl alloy powder absorbents, aimed at enhancing permeability in the decimeter-wave band for better absorption performance through Cr doping via wet ball-milling and subsequent annealing processes. The wet ball milling process facilitates the formation of a lamellar structure by inducing slip along shear stress in DO3 and α-Fe nanocrystals. During annealing, the introduced Cr element partially impedes the transition from the α-Fe phase to the DO3 phase, thereby amplifying the difference in magnetostrictive coefficients between these phases. Consequently, the flaky FeSiAlCr powders exhibit notably increased initial permeability and resonance frequency, particularly around 3 GHz, owing to domain rotation in the DO3 phase. In comparison to previously reported counterparts, the composite derived from these powders demonstrates a significant enhancement in the real part of effective permeability by approximately 66 %, alongside a 17 % reduction in density. Consequently, this composite exhibits a lowered reflection loss of below −5 dB within the frequency range of 0.7–3 GHz, reaching a minimum of −11 dB at 1.57 GHz, specifically with a thickness of 1.6 mm. These findings present an effective strategy for enhancing the magnetic permeability of alloy powders. The resultant microwave absorbing materials hold promising applications in stealth technology and wireless communication electronics.

High-loading cannabidiol powders for inhalation

Limited attempts have been made previously to develop high-loading CBD inhalable powders, which are essential for high dose delivery. Therefore, this study aimed to develop and characterise inhalable powders with ≥ 95 % w/w CBD by wet ball milling. The effects of magnesium stearate (2 % and 5 %) and inhaler resistance (low-resistance and high-resistance RS01 inhalers) on aerosol performance were also compared. Wet ball milling produced CBD powders with > 50 % production yield. The milled particles showed irregular shapes. The powders were crystalline with minimal amorphous content, low residual solvent level (<1%), and low moisture sorption (<4%). Magnesium stearate improved both the emitted and fine particle fractions. The aerodynamic particle size distribution of the formulations differed between the low-resistance and high-resistance RS01 inhalers. The latter decreased throat deposition but increased inhaler retention. The dissolution profiles showed that all three formulations released CBD steadily and plateaued at 30 min. The best scenario was CBD with 5 % magnesium stearate dispersed from the high resistance RS01 inhaler, showing the highest FPF with the lowest throat deposition. This combination may be tested in vivo in the future to investigate its pharmacokinetic profile.

Alternative processing routes on CsH2PO4 proton conductors: Cold sintering and ball-milling routes

Cesium dihydrogen phosphate (CsH2PO4) holds great potential as electrolyte for intermediate-temperature fuel cells and electrochemical devices due to its high proton conductivity (≥10−2 S/cm). This study reports on the variation of the microstructure of CsH2PO4 and its effect on its electrical and thermal properties, with special attention to the low-temperature conductivity behavior. To manipulate morphology, the particle size was decreased by wet ball-milling, while variations in grain growth were achieved by cold sintering. Above the superprotonic phase transition, the electrical conductivity was effectively independent of the grain size. Nonetheless, at lower temperatures, a brick layer analysis on the impedance data revealed that the conductivity of the monoclinic phase is governed by the conduction pathways along the parallel grain boundaries due to the humidified atmosphere. Overall, we propose two conduction mechanisms that could explain the grain boundary conductivity of these samples, revealing critical links between sample morphology and low-temperature electrical behavior.

In-situ coating strategy to synthesize ultra-soft sulfide solid-state electrolytes for dendrite-free lithium metal batteries

High energy density lithium metal batteries play a crucial role in future energy storage. High ionic conductivity argyrodite-type Li5.5PS4.5Cl1.5 is a promising candidate for future lithium metal all-solid-state batteries. However, under cold pressing conditions, the combination of high electronic conductivity and high porosity significantly accelerates the growth of lithium dendrites, resulting in low capacity and a short lifespan. In this study, we combined a simple wet ball milling and in-situ polymerization process to fabricate a polyvinylene carbonate-coated sulfide composite solid electrolyte. The ultra-soft particle, when cold-pressed without binders, completed a tightly packed and void-free internal structure. This electrolyte, combined with a stable LiF-rich interface layer on lithium metal, held a higher critical current density of 2.0 mA cm−2 than 0.65 mA cm−2 of uncoated argyrodite and a 2000-hour stable cycle at 0.5 mA cm−2 in lithium symmetric cells. The unique coating structure also mitigated the chemomechanical failure between electrolyte and electrode, preventing the rapid increase of interface impedance and achieving a high initial capacity of 173.5 mAh g−1 without a short circuit for 300 cycles in LiNi0.6Co0.2Mn0.2O2//Li cells.

Structure, magnetic properties and hyperthermia of Fe3-xCoxO4 nanoparticles obtained by wet high-energy ball milling

In this work, the methods of X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), Mössbauer spectroscopy (MS), magnetic properties measurements and specific loss measurements (hyperthermia) were used for the investigation of the structure and properties of Fe3-xCoxO4 nanoparticles. The Fe3-xCoxO4 nanoparticles were synthesized by using high-energy ball milling of Fe and Co mixed with water and surfactant additives. Co substitution increased the coercivity of the samples and changed the kinetics of oxidation process. The presence of cobalt ferrite was verified by MS. TEM images of synthesized samples demonstrated 5–50 nm particle size. Specific loss related heating effect depended mostly on the ratio between the samples coercivity and the amplitude of the high-frequency field. Specific loss power (SLP) and intrinsic loss power (ILP) values reached 164 W/g and 1.57 nH·m2/kg, respectively.

Atmosphere matters: The protection of wet ball milling instead of dry ball milling accelerates the electron transfer effect of sulfurized micron iron/biochar to Cr (VI)

Obstacles such as aggregation and low activity of micron zero-valent iron in pollutant treatment could be overcome by sulfidation and biochar support. Ball milling is a promising method for the preparation of iron-based composites but the milling atmosphere is critical. To maximize the reactivity and identify the effects of ball mill atmosphere, ball milling technology under wet and dry atmosphere was applied to prepare composites from mZVI, Na2S2O4, and pine wood biochar (BC) for Cr(VI) removal. The results showed that S-mZVI/BC-wet was highly dispersible with more FeS2 coverage and thus more efficient on Cr (VI) removal than S-mZVI/BC-dry (99.9 % removal in 80 min vs. 87.9 % removal in 24 h) at the optimum Fe: C mass ratio (1:1), S: Fe molar ratio (1:10), and reaction conditions. Cr(VI) was adsorbed by a spontaneous, endothermic mechanism that combined physisorption and chemisorption. The reduction process was vulcanization efficiency and iron cycle dependent. Reduction outperformed adsorption on the Cr(VI) removal and high reduction rateswere electron-selectively related (59.15 % for S-mZVI/BC-wet and 46.72 % for S-mZVI/BC-dry), implying S-mZVI/BC-wet was more capable. S-mZVI/BC-wet presented excellent anti-ageing property and slightly inferior regeneration performance. In conclusion, the composite prepared by wet ball milling have excellent performance in rapid and complete removal of Cr(VI), and S-mZVI/BC-wet has superior potential in acidic wastewater treatment.

Study on combustion characteristics and pyrotechnic cutting effects of bimetal thermite Ni/Al/Fe2O3 system

AbstractNano‐thermite has become a subject of significant interest in the composite energetic materials field due to its high energy release rate. To cater to diverse engineering needs, thermite formulations are often customized to fulfill specific criteria. This study investigates the potential of metal nickel (Ni) as an additive to modify nano‐thermite formulations, selected for its optimal calorific values and chemical reactivity. The base materials, nano‐aluminum (Al) and iron oxide (Fe2O3), are blended with varying mass ratios of Ni (1 %, 3 %, 5 %, 7 %, 9 %) using the wet ball milling method. Pre‐reaction and post‐reaction morphological and compositional alterations in the resultant thermite samples are scrutinized through SEM and XRD characterization tests. Moreover, DSC analysis and combustion experiments were conducted to examine the pyrolysis and combustion behaviors of the evaluated samples. The results reveal a reduced exothermic peak on the DSC curves with the introduction of Ni, making the liquid‐solid (L‐S) phase reaction more challenging compared to the Al/Fe2O3 thermite. Intriguingly, Ni addition progressively decreases the combustion temperature of thermites as the Ni's mass ratio increases, with a peak efficiency at 7 % in the perforation tests on stainless‐steel plates. This research further reveals that the thermite reaction mechanism is a combined consequence of the “pre‐ignition‐fusion” and “fusion‐diffusion” mechanisms. These insights can provide valuable guidance for designing thermite formulations for potential applications in storage, management, and pyrotechnic cutting areas.

Regional metakaolin particle size reduction for higher strength geopolymer

AbstractThe objective of this project was to further develop new composites and a testing program for the performance‐based specification for natural Amazonian geopolymer (GP) for use in ceramics and construction. While fly ash‐based alkali activated materials are now an established technology, metakaolin‐based GPs still need to be developed and optimized regarding the knowledge of the specific characteristics and properties of local resources. Amazonian kaolin was calcined into metakaolin (AMK). AMK particle size reduction for better reactive material was evaluated by means of dry and wet ball milling and sieving. Three types of metakaolin were analyzed for particle size distribution, and their size d50 ranged from 7.9 to 2.8 µm. Further GP characterization followed physical and mechanical properties in flexural strength tests. In addition, scanning electron microscopy and energy dispersive spectroscopy were used to investigate the microstructure of the materials. Energy dispersive X‐ray fluorescence was used to measure the GP material composition. Analysis of the results revealed that the strength and stiffness of sodium–metakaolin‐based GP were inversely proportional to particle size. All distinct particle size GPs showed, in general, some increase in strength and stiffness within curing times ranging from 3 to 28 days.

Influence of mixing technique on properties of Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte prepared by the solid-state reaction - A comparison of dry 3D mixing technique with wet ball-milling

Li1.3Al0.3Ti1.7(PO4)3 (LATP) NASICON(Na Super Ion Conductive)-type solid electrolyte is prepared using conventional wet ball-milling and dry 3D mixing techniques to investigate the influence of mixing technique on properties of LATP. The mixing techniques influence impurity formation of calcined LATP powder. Thus, sintering behavior of the calcined powders is also affected by the mixing technique, i.e. LiTiPO5 formation is confirmed in the ball-milling samples and Li-ion conductive Li4P2O7 is main impurity in the 3D mixing samples. The influence is not limited to impurity formation. Uniform grains are observed in the 3D mixing pellet, contrarily, non-uniform sintering occurs in the ball-milling sample. As a result, the 3D mixing pellets demonstrate higher Li-ion conductivity than the ball-mill samples. The dry 3D mixing technique, which can omit drying process, is promising for LATP preparation owing to simplification of preparation process and a formation of high Li-ion conductive LATP pellets. Also, this study clearly shows that the mixing techniques affect ionic conductivity of the sintered LATP significantly, emphasizing importance of mixing procedure in the solid-state reaction.

Impact of Grinding Balls on the Size Reduction of Aprepitant in Wet Ball Milling Procedure

One of the widely used approaches for improving the dissolution of poorly water-soluble drugs is particle size reduction. Ball milling is a mechanical, top-down technique used to reduce particle size. The effect of ball number, ball size and milling speed on the properties of milled Aprepitant is evaluated. A full factorial design was employed to investigate the influence of affecting factors on particle size reduction. The initial suspension was made by suspending the drug in distilled water using excipients followed by milling in a planetary ball mill. Ball size, ball number and milling speed modulated particle size distribution of Aprepitant. Increasing the number of balls from minimum to maximum for each ball size led to approximately a 28% reduction in mean particle size, a 37% decrease in D90%, and a 25% decrease in the ratio of volume mean particle diameter to numeric mean particle diameter. On average, using 10 mm balls instead of 30 mm balls reduced mean particle size by 1.689 µm. As a result, ball size, ball number, and milling speed are three effective factors in the process of ball milling. By increasing the ball number and decreasing the ball size, efficient micronization of drug particles takes place and the particle size is more uniform.

Effect of particle shape produced from wet ball milling on magnetic separation concentrate by fractal dimension

The particle shape in mineral processing is a function of the comminution mechanism. In this study, the effect of the concentrate particle shape, obtained from the wet ball milling and the low-intensity magnetic separator on magnetite ore is investigated by the fractal geometry approach. The particle shape is described by the fractal dimension, calculated by the divider method. The variable parameters of grinding time, loading ratio, and solid weight percentage were studied here. The fractal dimensions of the particles are obtained between 1.12 and 1.42. When the grinding time is increased from 45 to 65 minutes, the fractal dimension and product grades are increased from 1.19 to 1.42 and from 65.61 to 67.70%, respectively. By increasing the loading ratio from 14% to 22%, the fractal dimension and the product’s grades are increased from 1.17 to 1.38 and from 64.80 to 66.68%, respectively. By increasing the solid weight percentage from 35 to 55%, the fractal dimension and product grades are decreased from 1.32 to 1.12 and from 65.51 to 64.65%, respectively. The results show that the particle shape has a significant effect on the performance of the magnetic separator. It is the findings indicate a direct relationship between the particle fractal dimension and the grade of magnetic separation products.

Based on N, F, and P co-doping biomass carbon to construct 3D porous carbon coated LiFePO4 for preparing lithium-ion batteries

Because of its superior structural stability, high level of safety, and low cost, the olivine-type LiFePO4 (LFP) is a prevailing cathode material in lithium-ion batteries. However, its development is constrained to inferior electronic conductivity and sluggish diffusion kinetic. In this work, a biomass carbon source derived from microbial residue was introduced to modify LiFePO4 (LFP@NFPC). LFP@NFPC composite with three-dimensional (3D) porous structure was synthesized via a facile wet ball milling and high-temperature calcination. Through well-designed experiment and feasible data analysis, a high conductive 3D network structure is constructed by N, F, and P co-doped carbon coating in the surface of LiFePO4, facilitating fast electron transport and rapid reaction kinetics bewteen intercrystalline. Meanwhile, the LFP@NFPC with three-dimensional (3D) porous structure can also improve the accessibility of Li+ over a protrcated cycle. The as-prepared LFP@NFPC shows discharge specific capacities of 168.2, 138.4, and 103.8 mAh/g at 1, 10, and 50C, respectively. Simultaneously, the LFP@NFPC||Graphite full battery indicates a specific capacity of 161.2 mAh/g at 1C, thus exhibiting superior rate capacity and outstanding cycle stability. This work provides a sustainable and economical approach to modify the cathode material of LIBs.

Emulsification Characteristics of Insoluble Dietary Fibers from Pomelo Peel: Effects of Acetylation, Enzymatic Hydrolysis, and Wet Ball Milling.

To improve the application potential of pomelo peel insoluble dietary fiber (PIDF) in emulsion systems, acetylation (PIDF-A), cellulase hydrolysis (PIDF-E), and wet ball milling (PIDF-M) were investigated in this paper as methods to change the emulsification properties of PIDF. The impact of the methods on PIDF composition, structure, and physicochemical properties was also assessed. The results demonstrated that both acetylation modification and cellulase hydrolysis could significantly improve the emulsification properties of PIDF. The emulsions stabilized with PIDF-A and PIDF-E could be stably stored at 25 °C for 30 d without phase separation at particle concentrations above 0.8% (w/v) and had higher storage stability: The D4,3 increments of PIDF-A- and PIDF-E-stabilized emulsions were 0.98 μm and 0.49 μm, respectively, at particle concentrations of 1.2% (w/v), while the storage stability of PIDF-M-stabilized emulsion (5.29 μm) significantly decreased compared with that of PIDF (4.00 μm). Moreover, PIDF-A showed the highest water retention capacity (21.84 g/g), water swelling capacity (15.40 mL/g), oil retention capacity (4.67 g/g), and zeta potential absolute (29.0 mV) among the PIDFs. In conclusion, acetylation modification was a promising method to improve the emulsifying properties of insoluble polysaccharides.

Optimized Ilmenite Leachate by Wet Mechanical Activation for the Synthesis of TiO&lt;sub&gt;2&lt;/sub&gt; Nanoparticles through Sulfate Route

The extraction of ilmenite minerals using the sulfate route is one of the commercial methods for producing titanium dioxide (TiO2) materials. The sulfate process requires a high concentration of sulfuric acid to achieve high extraction yield of titanium. However, this process also results in the generation of high amounts of sulfuric acid waste. Modifying ilmenite minerals is thought to be one of approaches in reducing the consumption of highly concentrated sulfuric acid. In the current study, we investigated the effect of the ilmenite-to-water mass ratio (ITWR) on the wet-ball milling process to enhance the dissolution of titanium from the ilmenite mineral. The results revealed that increasing the water amount from 10 to 70% wt has decreased the particle size from 167.60 to 0.55 μm and increased the titanium yield from 479.36 to 1228.89 ppm. On the basis of investigation, it was shown there is a significant relationship between the ilmenite-to-water mass ratio and titanium dissolution, highlighting the importance of an optimal ratio for achieving maximum dissolving yield. The obtained TiO2 nanoparticles provide the average crystallite size of 4.16 nm, with rutile and anatase phase, and spherical morphology.