Hydrothermal treatment of pearl millet grains:Effects on nutritional composition,antinutrients and flour properties

Pearl millet(Pennisetum glaucum)is one of the major millets with high nutritional properties.This crop exhibits exceptional resilience to drought and high temperatures.However,the processing of pearl millet poses a significant challenge due to its high lipid content,enzyme activity,and presence of antinutrients.Consequently,it becomes imperative to enhance the quality and prolong the shelf life of pearl millet flour by employing suitable technologies.Hydrothermal treatment in the food industry has long been seen as promising due to its potential to reduce microbial load,inactivate enzymes,and improve nutrient retention.This study aims to investigate the effects of hydrothermal treatment on the quality characteristics of pearl millet.The independent variables of the study were soaking temperature(35,45,55℃),soaking time(2,3,4 h),and steaming time(5,10,15 min).Treatment conditions had a statistically significant effect on nutrient retention.Major antinutrients like tannins and phytates were reduced by 0.99% to 5.94% and 0.36% to 6.00%,respectively,after the treatment.Lipase activity decreased significantly up to 10% with the treatment conditions.The findings of this study could potentially encourage the use of pearl millet flour in the production of various food items and promote the application of hydrothermal treatment in the field of food processing.

Multi-Component Resource Recycling from Waste Light-Emitting Diode Under Hydrothermal Condition:Plastic Package Degradation,Speciation of Nano-TiO_(2),and Environmental Impact Assessment

Light emitting diodes(LEDs)have accounted for most of the lighting market as the technology matures and costs continue to reduce.As a new type of e-waste,LED is a double-edged sword,as it contains not only precious and rare metals but also organic packaging materials.In previous studies,LED recycling focused on recovering precious and strategic metals while ignoring harmful substances such as organic packaging materials.Unlike crushing and other traditional methods,hydrothermal treatment can provide an environment-friendly process for decomposing packaging materials.This work developed a closed reaction vessel,where the degradation rate of plastic polyphthalamide(PPA)was close to 100%,with nano-TiO_(2)encapsulated in plastic PPA being efficiently recovered,while metals contained in LED were also recycled efficiently.Besides,the role of water in plastic PPA degradation that has been overlooked in current studies was explored and speculated in detail in this work.Environmental impact assessment revealed that the proposed recycling route for waste LED could significantly reduce the overall environmental impact compared to the currently published processes.Especially the developed method could reduce more than half the impact of global warming.Furthermore,this research provides a theoretical basis and a promising method for recycling other plastic-packaged e-waste devices,such as integrated circuits.

The Impact of Hydrothermal Treatments on Technological Properties of Whole Grains and Soriz (<i>Sorghum oryzoidum</i>) Groats

Cereals and cereal products are the basic element in ensuring the food security of the population. Most cereal-based foods contain gluten. Nutritional therapy is the only treatment for people with gluten-related disorders. No gluten-free products are manufactured in the Republic of Moldova, and the imported ones are sold at very high prices. In this context, Moldova is an unexplored field and research is required. The paper investigated the impact of hydrothermal treatments on whole grains and sorghum groats. It was found that whole grains and sorghum groats have a cooking time of about 130 and 40 minutes, respectively, which can be reduced by about 2 times by prior hydration in water. Hydration media and their concentrations (NaCl solutions;sol. NaHCO3 and C6H8O7 concentrations 0.5%;1.0% and 2.0%) differently influence the cooking time, mass, volume and firmness of the grains.

Structural Changes of Y Zeolites with Different Initial SiO_2/Al_2O_3 Ratios during Hydrothermal Treatment

The effects of the initial framework SiO2/Al2O3 ratio and temperature on the structural changes of NaY zeolites during hydrothermal treatments are studied. Two samples with different framework SiO2/Al2O3 ratios are subjected to hydrothermal treatment at four different temperatures. For zeolite with a lower initial SiO2/Al2O3 ratio of 4.2, mesopores are easily formed because more framework aluminum is detached. Moreover, two kinds of mesopores are produced at a higher temperature due to the interconnection of vacancies and smaller mesopores. For zeolite with a higher initial SiO2/Al2O3 ratio of 6.0, there are less mesopores formed as compared with the lower initial SiO2/Al2O3 ratio sample, but there are some macropores formed. This may be attributed to the isolation of vacancies and the different distributions of aluminum in the crystal lattice of the zeolite. The experiment data show that NaY with the SiO2/Al2O3 ratio of 6.0 retains a high relative crystallinity during the hydrothermal treatment. This proves that a high framework SiO2/Al2O3 ratio benefits the stability of zeolite.

Effect of Dehulling and Hydrothermal Treatment on the Amino Acid Content of Soriz (<i>Sorghum oryzoidum</i>)

Cereals are the basic element in ensuring the food security of the population through the significant intake of carbohydrates, proteins, dietary fiber, vitamins and minerals. The processing of cereals leads to changes in their nutritional quality, which could lead to both reduced nutrients and anti-nutrients. Gluten-free cereal varieties attract attention as raw materials to improve the nutritional quality of food and to diversify the product range. Sorghum (Sorghum oryzoidum) is a hybrid of sorghum, obtained at the Institute for Scientific Research for Corn and Sorghum in the Republic of Moldova, by crossing Sudan grass (S. sudanense) and bicolor sorghum (S. bicolor). The research aimed to determine the impact of dehulling and hydrothermal treatment on the amino acid content of soriz. The obtained results reported that the dehulling and hydrothermal treatment led to the uneven modification of the amino acid content in the investigated samples. As a result of dehulling, the total amount of essential amino acids decreased by 19.8% compared to the native grain. Boiling whole grains without prior hydration led to 34% loss of essential amino acids compared to native grains, and pre-hydration of the grains and subsequent boiling reduced essential amino acid losses by 8% compared to cooked grains without hydration. Boiling grains with pre-hydration had a positive effect on the chemical index of lysine, methionine and cysteine, leucine and tryptophan. However, the nutritional quality of sorghum grain proteins and derivatives obtained, evaluated according to the chemical index, is low. The results obtained reported that dehulling and hydrothermal treatment unevenly altered the amino acid content, and the method of boiling grains with pre-hydration had a positive effect on the CSI of lysine, methionine and cysteine, leucine and tryptophan.

Breaking the temperature limit of hydrothermal carbonization of lignocellulosic biomass by decoupling temperature and pressure

Hydrothermal carbonization(HTC) of lignocellulosic biomass is a promising technology for the production of carbon materials with negative carbon emissions. However, the high reaction temperature and energy consumption have limited the development of HTC technology. In conventional batch reactors, the temperature and pressure are typically coupled at saturated states. In this study, a decoupled temperature and pressure hydrothermal(DTPH) reaction system was developed to decrease the temperature of the HTC reaction of lignocellulosic biomass(rice straw and poplar leaves). The properties of hydrochars were analyzed by scanning electron microscopy(SEM), Fourier transform infrared(FTIR) spectroscopy, X-ray photoelectron spectroscopy(XPS), Raman spectroscopy, X-ray diffraction(XRD), thermogravimetric analyzer(TGA), etc. to propose the reaction mechanism. The results showed that the HTC reaction of lignocellulosic biomass could be realized at a low temperature of 200℃ in the DTPH process, breaking the temperature limit(230℃) in the conventional process. The DTPH method could break the barrier of the crystalline structure of cellulose in the lignocellulosic biomass with high cellulose content, realizing the carbonization of cellulose and hemicellulose with the dehydration, unsaturated bond formation, and aromatization. The produced hydrochar had an appearance of carbon microspheres, with high calorific values, abundant oxygen-containing functional groups, a certain degree of graphitization, and good thermal stability. Cellulose acts not only as a barrier to protect itself and hemicellulose from decomposition, but also as a key precursor for the formation of carbon microspheres. This study shows a promising method for synthesizing carbon materials from lignocellulosic biomass with a carbon-negative effect.

Influence of Yttria Stabilized Zirconia and Hydrothermal Treatment on Plasma Sprayed Hydroxyapatite Coatings

A post-treatment of hydrothermal process was conducted to evaluate its effects on the material characteristics and mechanical properties of plasma-sprayed pure HA and HA/20% YSZ coatings.Surface morphology and microstructural changes,relative element contents as well as phase transformations were analyzed by scanning electron microscopy,energy dispersive spectroscopy,and X-ray diffractometry.Both microhardness and Young’s modulus were measured.CaCO3 was found existing before and after the whole process of post-treatment.Peaks of impurity phases such as CaO,TCP,and TTCP of as-sprayed coatings were observed to disappear while HA peaks show a tendency of getting higher and wider over time.Surface morphology of SEM analysis presents a clear deposition behavior of ultrafine HA crystallized particles and cross-sectional analysis exhibits a dense and fine structure.Mechanical properties of HA/20%YSZ coatings are found to be significantly higher than those of pure HA coatings and both of which displayed an overall increase with the heating time,indicating enhanced performances.

Effect of hydrothermal treatment on the carbon structure of Inner Mongolia lignite

Understanding the structural properties of lignite during hydrothermal treatment would aid in predicting the subsequent behavior of coal during the pyrolysis,liquefaction,and gasification processes.Here,hydrothermal treatment of Inner Mongolia lignite(IM)was carried out in a lab autoclave.The distribution of carbon in the lignite was monitored via solid 13C nuclear magnetic resonance spectroscopy,and the functional groups of oxygen in lignite were determined by Fourier transform infrared spectroscopy.The curve-fitting method was used to calculate the content of the functional groups quantitatively.The results show that hydrothermal treatment is an effective method for upgrading the lignite.The side chains of the aromatic ring in lignite are altered,while the main macromolecular structure remains nearly the same.The hydrothermal treatment of IM could be divided into three temperature-dependent stages.The first stage(<493 K)is the decomposition reaction of oxygen functional groups,where the O/C ratio decreases from 0.203 in raw IM to 0.185 for the IM treated at 493 K.In the second stage(493–533 K),hydrolysis of functional groups and hydrogen transfer between water and lignite occur.Here,the ratio of methylene to methyl increases from 0.871 in IM-493 to 1.241 for IM-533,and the content of quinone generates from the condensation of free phenol increased.The third stage(>533 K)involves breakage of the covalent bond,and the content of CH4 and CO in the emission gas clearly increase.

Influence of Hydrothermal Pre-Treatment of Coal Fly on the Synthesis of Belite Phase

In this paper, the results of an extensive investigation of hydrothermal pre-treatment for synthesizing belite phase from reactive mixtures （CaO/SiO2 molar ratio of 2） consisting of one waste kinds （bottom ash-BA or fly ash-FA） from fluidised brown coal combustion in Slovakian power plant and CaO （analytical grade reagent） addition are summarized. Changes in structure and phase composition of hydrothermally synthesized belite precursors and subsequent calcinated products were compared with those of starting mixtures. Based on XRD diffraction patterns, the formation of the new profiles corresponding to CSH phases with low degree of ordering as belite precursors after hydrothermal treatment was confirmed. Calcination of hydrotermally treated products at 900℃ led to transformation of CSH phases to wollastonite, belite and gehlenite phase. Differences in phase composition of products before and after calcination depend upon waste quality and precursor＇s synthesis conditions. Bottom ash isn＇t suitable as raw material for synthesizing belite phase because of high CaO content fixed in anhydrite form （44.1%）. Coal fly ash with low CaO content in anhydrite form （4.2%） and its hydrothermal treatment in combination with subsequent heating offer opportunities for the utilization of coal fly ash as raw material for belite production.

Optimization of Hydrothermal Treatment Parameters to Produce Chlorine-Free Alternative Solid Fuel from Plastic-Contained Municipal Solid Waste

An experimental study of the treatment of plastic-contained Japanese MSW （municipal solid waste） employing 1 ton capacity hydrothermal reactor to produce chlorine-free solid fuel has been performed. The system applies medium-pressure saturated steam at about 2 MPa in a stirred reactor for certain holding period. It was shown that the products exhibited organic chlorine conversion into inorganic chlorine, which can then be water washed. To obtain an optimal operating condition, the temperature and holding period was integrated into one parameter called RS （reaction severity）. It was found that to convert 75% organic chlorine in the MSW, the optimum RS number correlates to an operating temperature of about 225℃ and holding period of 90 min, or 235 ℃ for 60 min. Since hydrothermal treatment is a batch process, a shorter holding period is preferable to increase the number of batches and indirectly increase its processing capacity.

Reaction behaviour of Al_2O_3 and SiO_2 in high alumina coal fly ash during alkali hydrothermal process

The reaction behaviours of A1203 and SiO2 in high alumina coal fly ash under various alkali hydrothermal conditions were studied. The means of XRD, XRF, FTIR and SEM were used to measure the mineral phase and morphology of the solid samples obtained by different alkali hydrothermal treatments as well as the leaching ratio of SiO2 to A1203 in alkali solution. The results showed that with the increase of the hydrothermal treating temperature from 75 to 160 ~C, phillipsite-Na, zeolite A, zeolite P, and hydroxysodalite were produced sequentially while the mullite and corundum phase still remained. Zeolite P was massively formed at low-alkali concentration and the hydroxysodalite was predominantly obtained at high-alkali concentration. By the dissolution of aluminosilicate glass and the formation of zeolites together, the leaching efficiency of SiO2 can reach 42.13% with the mass ratio of A1203/SIO2 up to 2.19：1.

Facile hydrothermal synthesis of TiO_2-Ca P nano-films on Ti6Al4V alloy

Ti6Al4V alloy was subjected to hydrothermal treatment in the concentrated Ca3(PO4)2, Ca HPO4 and Ca(H2PO4)2 solutions for bioactive surface modification. The treated samples are covered by films composed of nano-particles with the size of 60-240 nm. Such film can also be grown on the strut surface of a Ti6Al4 V scaffold prepared by electron beam melting(EBM) technology. XPS analysis indicates that Ti element on the surface presents as TiO2, and Ca and P elements are in the form of calcium phosphate. XRD and Raman analyses show that the surface layer is composed of anatase TiO2 and hydroxyapatite. Potentiodynamic polarization test in a Ca-free Hank's balanced solution demonstrates that the treated sample has markedly improved corrosion resistance compared with the polished sample. The present work provides a bioactive surface modification method that is easily-operated, low-temperature, less corrosion, and applicable to porous Ti6Al4 V alloy for biomedical applications.

Luminescence properties of ZnS:Cu, Eu semiconductor nanocrystals synthesized by a hydrothermal process

ZnS：Cu, Eu nanocrystals with an average diameter of 80 nm are synthesized using a hydrothermal approach at 200 ℃. The photoluminescence （PL） properties of the ZnS：Cu, Eu nanocrystals before and after annealing, as well as the doping form of Eu, are studied. The as-synthesized samples are characterized by X-ray diffraction, scanning electron microscopy, inductively coupled plasma-atomic emission spectrometry, and the excitation and emission spectra （PL）. The results show that both Cu and Eu are indeed incorporated into the ZnS matrix. Compared with the PL spectrum of the Cu mono-doped sample, the PL emission intensity of the Cu and Eu-codoped sample increases and a peak appears at 516 nm, indicating that Eu3＋ ions, which act as an impurity compensator and activator, are incorporated into the ZnS matrix, forming a donor level. Compared with the unannealed sample, the annealed one has an increased PL emission intensity and the peak position has a blue shift of 56 nm from 516 nm to 460 nm, which means that Eu3＋ ions reduce to Eu2＋ ions, thereby leading to the appearance of Eu2＋ characteristic emission and generating effective host-to-Eu2＋ energy transfer. The results indicate the potential applications of ZnS：Cu, Eu nanoparticles in optoelectronic devices.

Characterization of Pr-CeO_2 Nano-crystallites Prepared by Low-temperature Combustion&Hydrothermal Synthesis

Pr-CeO2 Nano-crystalline red pigments were prepared by low-temperature combustion with a later hydrothermal treatment using Ce（NO3）3·6H2O and Pr6O11 as raw materials. The phase composition, coloring mechanism and morphology of pigments were analyzed by XRD, SEM, EDS and XPS. Results showed that Pr-CeO2 solid solution with a fluorite structure was obtained by the diffusion of Pr^＋3 into CeO2 crystal lattice during the synthesis process. XPS analysis indicated that Pr^＋3 substitutes Ce^＋4 in CeO2 and is compensated by oxygen vacancies. Compared with low-temperature combustion synthesis, the Pr-CeO2 pigments prepared with a subsequent hydrothermal treatment have an average grain size of about 16.70 nm, and the crystallinity and red tonality are improved.

Hydrothermal synthesis of zeolitic material from circulating fluidized bed combustion fly ash for the highly efficient removal of lead from aqueous solution

The utilization of coal fly ash derived from circulating fluidized bed combustion(CFBFA)still faces great challenges because of its unique characteristics.In this study,a zeolitic material with Na-P1 zeolite as the main phase was successfully synthesized via a hydrothermal method by using CFBFA as the raw material.The effects of hydrothermal temperature,time,and added CTAB amount on the characterizations of synthesized materials were investigated by XRD,SEM,and XPS.The properties of the optimal zeolitic material and its adsorption performance for Pb^(2+)in aqueous solution were evaluated.The influences of pH,initial concentration,dosage,and temperature on Pb^(2+)adsorption were also examined.Results revealed the following optimal parameters for the synthesis of zeolitic material:NaOH concentration of 2 mol·L^(-1),solid-to-liquid ratio of 1:10 g·ml^(-1),hydrothermal temperature of 110℃,hydrothermal time of 9 h,and CTAB amount of 1 g(per 100 ml solution).The adsorption capacities of the zeolitic material reached 329.67,424.69,and 542.22 mg·g^(-1) when the pH values of aqueous solution were 5,6,and 7,respectively.The Pb^(2+)removal efficiency can reach more than 99%in aqueous solution with the initial concentrations of 100-300 mg·L^(-1) under pH 6 and suitable adsorbent dosage.The adsorption and kinetics of Pb^(2+)on the zeolitic material can be described by Langmuir isotherm and pseudo-second-order kinetic models,respectively.The ion exchange between Pb^(2+)and Na^(+)and chemisorption are the main adsorption mechanism.All these findings imply that the synthesis of low-cost adsorbent for Pb^(2+)removal from weak acid and neutral aqueous solution provides a highly effective method to utilize CFBFA.

Dealumination kinetics of composite ZSM-5/mordenite zeolite during steam treatment: An in-situ DRIFTS study

To get a better understanding of structural deactivation of ZSM-5/MOR during the catalytic cracking of n-heptane in the steam atmosphere, a comprehensive mechanism of hydrothermal dealumination was proposed through in-situ diffuse reflectance Fourier transform infrared spectroscopy(DRIFTS) in this work. The mechanism can be divided into two steps: firstly, the hydrolysis of four Al\\O bonds, and secondly, the self-healing of Si\\OH bonds accompanied with partial condensation of the extra-framework Al species. Accordingly, the kinetics of dealumination process has also been fully discussed. In the IR spectra, the range of 3450–3850 cm^(-1) could be deconvolved to distinguish the hydroxyl groups on the different position and calculate the consumption of each hydroxyl group during the reaction. Based on results from the in-situ DRIFTS, the kinetics of dealumination was hence developed and also in well agreement with the kinetics of deactivation of ZSM/MOR catalysts during the reaction in the presence of little coke deposits.

Nature of Surface Layer and Electrochemical Behavior of NaOH Hydrothermally Treated NiTi Alloy

NiTi samples were hydrothermally treated in NaOH at 200℃ with different soaking times. The morphology of the surface layer formed was studied by scanning electron microscopy (SEM). The composition of the layer and the major phases present were determined by energy-dispersive spectroscopy (EDS) and X-ray diffractometry (XRD), respectively. In contrast to the results reported by some authors, the surface layer was essentially Ni(OH)2 instead of being TiO2. The electrochemical behavior of the samples was studied by electrochemical impedance spectroscopy (EIS) in 3.5% NaCl solution at 23℃, and analyzed using a simplified Randle circuit consisting of a resistance R and a capacitance C in parallel. After hydrothermal treatment, R was increased by a factor ranging from 1.5 to 5.0 times, depending on the treatment time. The value of R of all the samples became steady within a period of less than 15 h. Results of the present study indicate that alkaline treatment leads to the growth of an insulating layer on NiTi, but the method is not suitable for surface modification of NiTi implants due to the enhanced Ni content in the surface layer.

Performances of lithium manganese oxide prepared by hydrothermal process

A simple hydrothermal process followed by heat treatment was applied to the preparation of spinel Li1.05Mn1.95O4. In this process, electrolytic manganese dioxide(EMD) and LiOH·H2O were used as starting materials. The physiochemical properties of the synthesized samples were investigated by thermogravimetry-differential scanning calorimetry(TG-DSC), X-ray diffractometry(XRD), and scanning electronic microscopy(SEM). The results show that the hydrothermally synthesized precursor is an essential amorphous. The precursor can be easily transferred to spinel powders with a homogeneous structure and a regularly-shaped morphology by heat treatment. Li1.05Mn1.95O4 powder obtained by heat treating the precursor at 430 °C for 12 h and then calcining at 800 °C for 12 h shows an excellent cycling performance with an initial charge capacity of 118.2 mA·h·g-1 obtained at 0.5C rate and 93.8% of its original value retained after 100 cycles.

Innovative construction of macroporous–mesoporous structured spherical alumina and its hydrothermal stability

The pore structure of spherical alumina supports is closely related to the dispersion of catalytically active components and the diffusion of reactants.Maintaining excellent pore structure under strict reaction conditions is of utmost importance.In this work,sphericalγ-Al_(2)O_(3)support with a bimodal pore structure,composed of macropores and mesopores,was successfully synthesized using dodecane as the pore-forming agent through the oil–ammonia column-shaping method.The morphology and internal pore structure of the alumina were found to be influenced by the amount of surfactant added and ultrasound treatment conditions.Notably,when concentration of surfactant was 4‰and ultrasound voltage of 20 V was applied,the resultingγ-Al_(2)O_(3)-4‰-20 displayed a highly concentrated distribution of macropores with an average pore size of 100 nm,resulting in an impressive porosity of 69.21%.In contrast,the untreated sample ofγ-Al_(2)O_(3)-0-0 only exhibited a mesoporous distribution with a porosity of 54.03%.Moreover,after being subjected to a hydrothermal treatment in a high temperature(600°C)and high humidity(water vapor)environment for 120 h,theγ-Al_(2)O_(3)-4‰-20 sample maintained a high BET specific surface area of 170.9 m^(2)g^(−1)and mercury intrusion porosimetry specific surface area of 263.3 m^(2)g^(−1).

Effects of ball milling time on porous Ti-3Ag alloy and its apatite-inducing abilities

Ti and Ag powders were mixed with different ball milling time （1, 2, 5 and 10 h） and sintered into porous Ti-3Ag alloys. The samples were treated with hydrothermal treatment, and their apatite-inducing abilities were further evaluated by immersion in modified simulated body fluid. The results indicate that the high surface energy brought by powder refinement leads to the decline of Ag, but promotes the oxidation of Ti during the sintering process. Meanwhile, the hydrothermal treated porous Ti-3Ag alloys prepared by the powders ball milled for 10 h possess the best apatite-inducing ability.