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.

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.

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.

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.

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.

Effects of ammonia concentration in hydrothermal treatment on structure and redox properties of cerium zirconium solid solution

Cerium zirconium solid solution is a key washcoat material for automotive three-way catalysts(TWCs).However,improving the redox ability and high temperature thermal stability of cerium zirconium solid solution is still a challenge.In this paper,the cerium zirconium solid solution was prepared by a coprecipitation-hydrothermal method,and the effects of the ammonia concentration on their structures and redox properties were investigated.The results show that when the ammonia concentration is 0.8 mol/L,the aged sample(1100℃/10 h)of cerium zirconium solid solution has the highest specific surface area of 23.01 m^(2)/g.Additionally,the increase of ammonia concentration improves the uniformity of phase compositions and increases the oxygen vacancies.When the ammonia concentration reaches 0.4 mol/L,the cerium zirconium solid solution exhibits the best redox activity,with the lowest reduction temperature of 565℃.Therefore,increasing ammonia concentration in the hydrothermal treatment is beneficial to the thermal stability and redox performance of cerium zirconium solid solution.

Layered double hydroxide using hydrothermal treatment： morphology evolution, intercalation and release kinetics of diclofenac sodium

The present work demonstrates the possibilities of hydrothermal trans- formation of Zn-AI layered double hydroxide （LDH） nanostructure by varying the synthetic conditions. The manipulation in washing step before hydrothermal treatment allows control over crystal morphologies, size and stability of their aqueous solutions. We examined the crystal growth process in the presence and the absence of extra ions during hydrothermal treatment and its dependence on the drug （diclofenac sodium （Dic- Na）） loading and release processes. Hexagonal plate-like crystals show sustained release with -90% of the drug from the matrix in a week, suggesting the applicability of LDH nanohybrids in sustained drug delivery systems. The fits to the release kinetics data indicated the drug release as a diffusion-controlled release process. LDH with rod-like morphology shows excellent colloidal stability in aqueous suspension, as studied by photon correlation spectroscopy.

Preparation of Oriented Barium Titanate Thin Films by Combination of Electrophoretic Deposition with Hydrothermal Treatment

Highly oriented barium titanate （BaTiO 3） thin films on Pt substrate were fabricated by combination of electrophoretic deposition with hydrothermal treatment.The structure and morphology of thin films were characterized by X-ray diffraction and field-emission scanning electron microscopy.It is found that the titania precursor film,Ba（OH）2 concentration and hydrothermal temperature play crucial roles in the film morphology and orientation.The BaTiO3 thin films with highly （110） preferred orientation can be formed on polycrystalline Pt substrate by appropriate adjustment of the reaction conditions.The orientation parameter f of highly oriented BaTiO3 films was up to 1.00.The films exhibited a smooth and crack-free surface and remained in the layered structure.In situ topotactic transformation and dissolution-crystallization mechanisms were proposed to explain the morphology and orientation of BaTiO3 films during hydrothermal treatment.

Understanding Formation Mechanism of Titanate Nanowires through Hydrothermal Treatment of Various Ti-Containing Precursors in Basic Solutions

Titanate nanowires prepared by hydrothermal treatment of Ti02 in NaOH solution have attracted intensive attentions, but the formation mechanism is still under debate. Herein, we report an in-depth study on the formation mechanism through investigating the hydrothermal behavior of various Ti-containing precursors in basic solutions, including Ti, TiN, TiO2, Ti2SnC and Ti2AIN. Based on the results by means of X-ray diffraction （XRD）, transmission electron microscopy （TEM） and Raman spectroscopy, it is demonstrated that the crystal structure of the hydrothermal products is irrespective to the structure of the precursors or the types of basic solution （NaOH or KOH） in use. Alkali ions play an important role in the formation of titanate nanowires. The formation mechanism of the resultant titanate nanowires was proposed to be dissolution-crystallization mechanism.

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.

Liquid-phase a-Pinene Isomerization over Fe-doped Sulfated Zirconia Prepared by a Hydrothermal Treatment-assisted Process

A series of Fe-doped （0.5%--3%） sulfated zirconia have been prepared by a hydrothermal treatment-assisted process. Textural and structural characterizations of the as-synthesized materials were performed by means of N2 adsorption, X-ray diffraction, transmission electron microscopy, scanning electron microscopy and thermogravimetric analysis. Temperature-programmed desorption of ammonia was used to determine the acidity of the samples. The effects of Fe-doping on the structure, acidity and catalytic activity of sulfated zirconia for liquid-phase a-pinene isornerization were investigated. The incorporation of small amounts of Fe into sulfated zirconia results in the increase of sulfate content and the number of acid sites, which is responsible for the enhanced activity of Fe-doped catalysts in comparison with the undoped one. Meanwhile, hydrothermal treatment helps to improve the activity of the catalyst.

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.

Formation and Bioactivity of SrTiO_3 Nanotubes on Titanium by Modified Anodization and Hydrothermal Treatment

SrTiO3 nanotube films with good adhesion strengths to Ti substrates were fabricated by using a hybrid approach with a modified anodization and a hydrothermal treatment （HT）. The effect of Sr^2＋ concentration in HT solutions on the morphologies and phase components of the nanotubes were investigated, the SrTiO3 nanotubes formation mechanism was explored, and the adhesion strengths, hydrophilicity and apatite-forming ability of the SrTiO3 nanotubes were also evaluated. The results demonstrated that with increasing the incorporation of Sr^2＋ into the nanotubes, no obvious changes of the lengths and outer diameters of the nanotubes were observed, but the wall thickness and the crystallinity of SrTiO3 in the nanotubes increased. The accumulation of Sr at the inner tube wall indicated that the reaction of Sr^2＋ with TiO2 mainly occurred in the vicinity of internal surfaces of the closely arranged nanotubes. The formation of the SrTiO3 nanotubes could be attributed to an in situ dissolution-recrystallization process. The SrTiO3 nanotubes exhibited good hydrophilicity and bioactivity, and the induced apatite preferred to nucleate on the nanotubes with higher crystallinity and Sr content, indicating a good hio-adaptability of the SrTiO3 nanotubes for orthopedic application.

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.