Fe(PyTACN)‐Catalyzed cis‐Dihydroxylation of Olefins with Hydrogen Peroxide

A family of iron complexes with general formula [Fe(II)(^R,Y,XPyTACN)(CF₃SO₃)₂], where ^R,Y,XPyTACN=1‐[2′‐(4‐Y‐6‐X‐pyridyl)methyl]‐4,7‐dialkyl‐1,4,7‐triazacyclononane, X and Y refer to the groups at positions 4 and 6 of the pyridine, respectively, and R refers to the alkyl substitution at N‐4 and N‐7 of the triazacyclononane ring, are shown to be catalysts for efficient and selective alkene oxidation (epoxidation and cis‐dihydroxylation) employing hydrogen peroxide as oxidant. Complex [Fe(II)(^Me,Me,HPyTACN)(CF₃SO₃)₂] ( 7 ), was identified as the most efficient and selective cis‐dihydroxylation catalyst among the family. The high activity of 7 allows the oxidation of alkenes to proceed rapidly (30 min) at room temperature and under conditions where the olefin is not used in large amounts but instead is the limiting reagent. In the presence of 3 mol% of 7 , 2 equiv. of H₂O₂ as oxidant and 15 equiv. of water, in acetonitrile solution, alkenes are cis‐dihydroxylated reaching yields that might be interesting for synthetic purposes. Competition experiments show that 7 exhibits preferential selectivity towards the oxidation of cis olefins over the trans analogues, and also affords better yields and high [syn‐diol]/[epoxide] ratios when cis olefins are oxidized. For aliphatic substrates, reaction yields attained with the present system compare favourably with state of the art Fe‐catalyzed cis‐dihydroxylation systems, and it can be regarded as an attractive complement to the iron and manganese systems described recently and which show optimum activity against electron‐deficient and aromatic olefins.     

Facile preparation of a silica‐sphere–poly(catechol hexamethylenediamine) composite for the competitive removal of cadmium(II), lead(II), and copper(II) ions

A silica‐sphere–poly(catechol hexamethylenediamine) (PCHA–SiO₂) composite was prepared via the one‐step facile polymerization of catechol and hexamethylenediamine; this method uses a silica sphere as a hard template. The chemical structures and morphologies of this composite were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, and transmission electron microscopy. The adsorption experiments indicated that the PCHA–SiO₂ composite served as a very attractive adsorbent for Pb(II)‐, Cu(II)‐, and Cd(II)‐ion removal at lower concentrations and had very good selective adsorption abilities for Pb(II) and Cu(II) ions in a solution contaminated with these three ions at higher concentrations. These interesting results may have been due to the reversible H⁺ adsorption–desorption properties of the characteristic phenol amine structure of the PCHA–SiO₂ composite. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45839.     

Influence of ionic speciation on electrocatalytic performance of polyaniline coated platinum electrode: Fe(III)/Fe(II) redox reaction

Porous-polyaniline coated Pt electrode (PANI/Pt) was electro-synthesized potentiodynamically in 0.1 M aniline + 0.5 M H₂SO₄ and morphologically characterized by scanning electron microscopy (SEM). Nature of predominant Fe-species in HCl and H₂SO₄ was checked by UV-vis spectrophotometry. Electrocatalysis of Fe(III)/Fe(II) reaction was studied by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) for three different solution compositions viz. (i) FeCl₃/FeCl₂ in 1 M HCl, (ii) FeCl₃/FeCl₂ in 0.5 M H₂SO₄ and (iii) Fe₂(SO₄)₃/FeSO₄ in 0.5 M H₂SO₄. For different thicknesses of PANI, the peak current increased irrespective of the nature of the Fe-species, but the polarity of the charge on the Fe-species showed great influence on reversibility of electrocatalysis by PANI/Pt. The Donnan interaction of the polyaniline modified electrode for the three compositions was investigated with respect to [Fe(CN)₆]³⁻/H₂[Fe(CN)₆]²⁻ which are believed to be the predominant species present in K₃[Fe(CN)₆]/K₄[Fe(CN)₆] solution in 0.5 M H₂SO₄. The electrocatalytic performance of PANI/Pt for Fe(III)/Fe(II) redox reaction was found superior in HCl compared to that in H₂SO₄.     

Highly efficient separation of methane from nitrogen on a squarate‐based metal‐organic framework

Highly selective capture of methane from nitrogen is considered to be a feasible approach to improve the heating value of methane and mitigate the effects of global warming. In this work, an ultramicroporous squarate‐based metal‐organic framework (MOF), [Co₃(C₄O₄)₂(OH)₂] (C₄O₄^2? = squarate), with enhanced negative oxygen binding sites was synthesized for the first time and used as adsorbent for efficient separation of methane and nitrogen. Adsorption performance of this material was evaluated by single‐component adsorption isotherms and breakthrough experiments. Furthermore, density functional theory calculation was performed to gain the deep insight into the adsorption binding sites. Compared with the other state‐of‐the‐art materials, this material exhibited the highest adsorption selectivity (8.5–12.5) of methane over nitrogen as well as the moderate volumetric uptake of methane (19.81 cm³/cm³) under ambient condition. The unprecedented selectivity and chemical stability guaranteed this MOF as a candidate adsorbent to capture CH₄ from N₂, especially for the unconventional natural gas upgrading. © 2018 American Institute of Chemical Engineers AIChE J, 64: 3681–3689, 2018     

Preparation and properties of a form‐stable phase‐change hydrogel for thermal energy storage

In this study, we aimed to fabricate a form‐stable phase‐change hydrogel (PCH) with excellent mechanical properties and heat‐storage properties. Sodium alginate (SA) and polyacrylamide (PAAm) composite hydrogels were prepared with ionically crosslinked SA in a PAAm hydrogel network. Glauber's salt [i.e., sodium sulfate decahydrate (Na₂SO₄·10H₂O)] was incorporated within the hydrogel network as a phase‐change material. Scanning electron microscopy micrographs revealed that Na₂SO₄·10H₂O was confined in the micropores of the hydrogel inner spaces, and differential scanning calorimetry curves showed that the composite hydrogel possessed a considerable storage potential. Mechanical properties tests, such as tensile and compressive measurements, presented a decreasing trend with increasing Na₂SO₄·10H₂O dosage. We concluded that the prepared composite PCH could be used to design hydrogel materials with thermal‐energy‐storage applications. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43836.     

Local reactivity of diamond-like carbon modified PTFE membranes used in SO2 sensors

The local electrochemical activity of polytetrafluorethylene (PTFE) membranes coated with diamond-like carbon (DLC) was investigated using scanning electrochemical microscopy (SECM). During z-approach curves in the feedback mode of SECM unexpected local variations in the electron-transfer rate of [Fe(CN)₆]^3−/4− and [Ru(NH₃)₆]^3+/2+ were observed. This local heterogeneity of the electrochemical activity was further evaluated in a system adapted from SO₂ gas sensors. In this case, the Cu^2+/+ couple is used as dissolved reversible redox system. Reaction of SO₂ with Cu²⁺ yields Cu⁺ which is re-oxidized at the DLC-coated PTFE membrane. Gas permeation/tip-collection mode SECM experiments allowed visualizing the local pore distribution as sites where the SO₂ is permeating through the membrane and hence formation of Cu⁺ takes place.     

Synthesis and characterization of magnetic beads containing aminated fibrous surfaces for removal of Reactive Green 19 dye: kinetics and thermodynamic parameters

BACKGROUND: Poly(HEMA‐co‐MMA) beads were prepared from 2‐hydroxyethyl‐methacrylate (HEMA) and methylmethacrylate (MMA) in the presence of FeCl₃. Thermal co‐precipitation of Fe(III) ions containing beads with Fe(II) ions was carried out under alkaline conditions. The magnetic beads were grafted with poly(glycidylmethacrylate; p(GMA)), and the epoxy groups of the grafted p(GMA) brushes were converted into amino groups by reaction with ammonia. RESULTS: The magnetic beads were characterized by surface area measurement, electron spin resonance (ESR), Mössbauer spectroscopy and scanning electron microscopy (SEM). The maximum adsorption of Reactive Green‐19 (RG‐19) dye on the p(GMA) grafted and amine modified magnetic beads was around pH 3.0. The adsorption capacity of magnetic beads was 84.6 mg dye g^?1. The effects of adsorbent dosage, ionic strength and temperature have also been reported. Batch kinetic sorption experiments showed that a pseudo‐second‐order rate kinetic model was applicable. CONCLUSION: The p(GMA) grafted and amine modified magnetic beads (adsorbent) were expected to have the advantage of mobility of the grafted chains in the removal of acidic dyes from aqueous solutions. The magnetic beads have potential as an adsorbent for removal of pollutants under various experimental conditions without significant reduction in their initial adsorption capacity. Copyright © 2011 Society of Chemical Industry     

Synthesis of cationic nickel(II) compounds for butadiene polymerization

A series of cationic nickel(II) compounds with various counter ions ([BF₄]^–, [CF₃SO₃]^–) and N‐bearing ligands (1,10‐phenanthroline, benzimidazole and terpyridine) were synthesized. The simple compound, Ni(Phen)₂Cl₂, was prepared as a reference compound. All title compounds were characterized by elemental analysis, and infrared spectra analyses and compounds, some specific ones, were further examined by X‐ray crystallographic analysis. Upon treatment with ethylaluminum sesquichloride, these nickel(II) compounds exhibited high activities (up to 88.5%/4 h) for butadiene polymerization and afforded liquid polybutadiene (M_w < 30,000) with a high cis‐content (up to 92.1%). Various polymerization conditions were investigated in detail, and it was found that less steric hindrance of the ligands enhanced the catalytic activities of the nickel(II) compounds. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40511.     

Biosorption of phenolic compounds from aqueous solutions onto chitosan–abrus precatorius blended beads

BACKGROUND: This research focuses on understanding the biosorption process and developing a cost‐effective technology for the treatment of water contaminated with phenolic compounds (phenol, 2‐chlorophenol and 4‐chlorophenol), which are discharged into the aquatic environment from a variety of sources and are highly toxic. In order to remove phenolic compounds from water, a new biobased sorbent is developed, blending chitosan with abrus precatorius, both naturally occurring biopolymers. The resulting chitosan–abrus precatorius blended beads (CS/Ab) were characterized by Brunauer, Emmett and Teller (BET) analysis, Fourier Transform Infrared (FTIR) spectroscopy and scanning electron microscopy (SEM) techniques under batch equilibrium and column flow experimental conditions. The binding capacity of the biosorbent was investigated as a function of initial pH, contact time, initial concentration of adsorbate and dosage of adsorbent. RESULTS: The percentage removal of phenol, 2‐CP and 4‐CP increased with increasing adsorbent dose, while the adsorption capacity at equilibrium, q_e (mg g^?1) (amount of phenol, 2‐CP and 4‐CP loaded per unit weight of adsorbent) decreased. The equilibrium time was found to be 240 min for full equilibration of all adsorbates. Adsorption kinetic and isotherm studies showed that the pseudo‐first‐order model and the Langmuir isotherm were the best choices to describe the adsorption behaviors. The maximum monolayer adsorption capacity of phenol, 2‐CP and 4‐CP on to the (CS/Ab) beads was found to be 156 mg g^?1, 204 mg g^?1 and 278 mg g^?1, respectively. CONCLUSION: The experimental results suggested that (CS/Ab) blended beads are effective in the removal of phenolic compounds from aqueous medium. Copyright © 2009 Society of Chemical Industry     

Removal of heavy metal ions from aqueous solutions by radiation‐induced chitosan/(acrylamidoglycolic acid‐co‐acrylic acid) magnetic nanopolymer

An effective method was developed to isolate toxic heavy metal ions from the aqueous solution by the magnetic nanopolymers. The magnetic sorbent was prepared with radiation‐induced crosslinking polymerization of chitosan (CS), 2‐acrylamido‐glycolic acid (AMGA), and acrylic acid (AAc), which stabilized by magnetite (Fe₃O₄) as nanoparticles. The formation of magnetic nanoparticles (MNPs) into the hydrogel networks was confirmed by Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, and Scanning electron microscopy, which revealed the formation of MNPs throughout the hydrogel networks. The swelling behavior of the hydrogels and magnetic ones was evaluated at different pH values. The adsorption activity for heavy metals such as Cu²⁺ and Co²⁺ by nonmagnetic and magnetic hydrogels, Fe₃O₄/CS/(AMGA‐co‐AAc), in terms of adsorption amount was studied. It was revealed that hydrogel networks with magnetic properties can effectively be used in the removal of heavy metal ions pollutants and provide advantageous over conventional ones. POLYM. ENG. SCI., 55:1441–1449, 2015. © 2015 Society of Plastics Engineers     

A redox poly(ionic liquid) hydrogel: Facile method of synthesis and electrochemical sensing

In this article, a redox-responsive poly(ionic liquid) (redox-PIL) hydrogel Poly(1-vinyl-3-propionate imidazole phenothiazine sulfonic acid)-chitosan [Poly(VPI⁺PTZ-(CH₂)₃SO₃⁻)-CS] was produced by using chitosan (CS) crosslinking with redox-PIL Poly(1-vinyl-3-propionate imidazole phenothiazine sulfonic acid [Poly(VPI⁺PTZ-(CH₂)₃SO₃⁻)]. The incorporation of redox-active counter anions 3-(phenothiazine-10-yl) propane 1-sulfonic acid anions (PTZ-(CH₂)₃SO₃⁻) into cationic PIL-polyimidazole rendered Poly(VPI⁺PTZ-(CH₂)₃SO₃⁻) with electron catalytic ability, ionic conductivity, and electron conductivity. Poly(VPI⁺PTZ-(CH₂)₃SO₃⁻)-CS combines the properties of hydrogel and redox-PIL, thus offering intrinsic porous conducting frameworks and promoting the transport of charges, ions, and molecules, leading hydrogel with excellent electrochemical properties. The crosslinking occurrence of Poly(VPI⁺PTZ-(CH₂)₃SO₃⁻) and CS resulting from the synthetic process of hydrogel was verified by differential scanning calorimetry and thermogravimetric analysis. A three-dimensional polymer network hydrogel with good biocompatibility and permeability was formed after crosslinking. In addition, only 64% weight loss within 600 °C was observed in Poly(VPI⁺PTZ-(CH₂)₃SO₃⁻)-CS representing its thermally stable performance. When used as an electrochemical sensor, the hydrogel-modified gold electrode improved the electrocatalytic oxidation of cysteine. Differential pulse voltammetry results indicated that the detection range was from 5 × 10⁻⁸ to 5 × 10⁻³ M and the limit of detection was 6.64 × 10⁻⁸ M. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 48051.     

Preparation and performance evaluation of composite hollow fiber membrane for SO2 separation

Emission of sulfur dioxide (SO₂) from coal power plants has to be controlled and minimized to reduce environmental risk. This study aimed to investigate the hollow fiber composite membrane was used for the removal of SO₂ from a SO₂/CO₂/N₂ mixed gas. Moreover, for the improvement of SO₂ removal efficiency, the polyetherimide (PEI) membrane was coated with poly(vinyl chloride)‐graft‐poly(oxyethylene methacrylate) (PVC‐g‐POEM). The PVC‐g‐POEM/PEI composite hollow fiber membrane was extensively characterized by various techniques including scanning electron microscopy, Fourier transform infrared spectroscopy, and atomic force microscopy. Experiments with permeation of SO₂, CO₂, N₂, and a ternary gas mixture were carried out to observe membrane behavior in response to different operating conditions. As a result, permeance of SO₂ was 105–2705 GPU and selectivity of SO₂/CO₂ was 3.9–175.6. From the mixed gas separation experiment, the maximum SO₂ removal efficiency reached up to 84.5%. © 2014 American Institute of Chemical Engineers AIChE J, 60: 2298–2306, 2014     

Ethylammonium nitrate enhances the extraction of transition metal nitrates by tri-n-butyl phosphate (TBP)

Several molecular polar solvents have been used as solvents of the more polar phase in the solvent extraction (SX) of metals. However, the use of hydrophilic ionic liquids (ILs) as solvents has seldomly been explored for this application. Here, the hydrophilic IL ethylammonium nitrate (EAN), has been utilized as a polar solvent in SX of transition metal nitrates by tri-n-butyl phosphate (TBP). It was found that the extraction from EAN is considerably stronger than that from a range of molecular polar solvents. The main species of Co(II) and Fe(III) in EAN are likely [Co(NO₃)₄]²⁻ and [Fe(NO₃)₄]⁻, respectively. The extracted species are likely Fe(TBP)₃(NO₃)₃ and a mixture of Co(TBP)₂(NO₃)₂ and Co(TBP)₃(NO₃)₂. The addition of H₂O or LiCl to EAN reduces the extraction because the metal cations coordinate to water molecules and chloride ions stronger than to nitrate ions. This study highlights the potential of using hydrophilic ILs to enhance SX of metals.     

Removal of SO2 Using a Magnetically Fluidized Bed in the Semi‐Dry Flue Gas Desulfurization Process: Roles of Ferromagnetic Particles and Applied Magnetic Field in the Desulfurization Reaction

A new semidry flue gas desulfurization (FGD) process is proposed. The process uses a magnetically fluidized bed (MFB) as the reactor in which ferromagnetic particles are fluidized with simulated flue gas under the influence of an external magnetic field. A slurry of lime is continuously sprayed into the reactor by an atomizer fixed at the top of the bed. As a consequence, the desulfurization reaction and slurry drying take place simultaneously in a same reactor. Experiments with a laboratory‐scale apparatus were carried out to investigate the roles of the ferromagnetic particles and the magnetic field applied in the desulfurization reaction. The results show that when ferromagnetic particles are used as the fluidization material, both sulfite (SO₃^2–) salts and sulfate (SO₄^2–) salts are found in the desulfurization products. When quartz particles are used, only sulfite (SO₃^2–) salts are found. This suggests that the Fe(III) ions and Fe(II) ions result from the ferromagnetic particles dissolving in the liquid phase. In addition, the ions act as catalysts in the oxidation of S(IV) to S(VI) and react with SO₂ producing FeSO₃ and Fe₂(SO₄)₃ as the products. On the other hand, the level of the sulfate (SO₄^2–) salts in the products increases with increasing intensity of applied field intensity, which suggests that the oxidation of S(IV) can be enhanced by the applied magnetic field. The oxidation of S(IV) can increase the solubility of SO₂, and therefore, intensify the reaction between SO₂ and Ca(OH)₂, leading to an increased SO₂ removal efficiency.     

Synthesis and Characterization of Hydrazinium Azide Hydrazinate

Hydrazinium azide hydrazinate, [N₂H₅]⁺[N₃]⁻ċN₂H₄ was synthesized from equimolar amounts of hydrazinium azide and hydrazine and characterized by single crystal X‐ray diffraction: monoclinic, P 2₁/c, a=6.3704(2), b=12.1111(4), c=6.9940(2) Å, β=91.8666(2) °, V=539.32(3) ų, Z=4, ρ=1.320 g cm⁻¹. The compound is less hygroscopic and less volatile than hydrazinium azide. Explosion of [N₂H₅]⁺[N₃]⁻ċN₂H₄ yielded dinitrogen (N₂), ammonia (NH₃) and dihydrogen (H₂). Compared to hydrazinium azide, the hydrazine adduct produces larger amounts of ammonia in the explosion.     

Fabrication and characterization of hybrid films based on polyaniline and graphitic carbon nitride nanosheet

Hybrid films of polyaniline/graphitic carbon nitride (PANI/g‐C₃N₄) deposited on titanium was fabricated. First, g‐C₃N₄ as a two‐dimensional graphite‐like structure was synthesized by the stepwise condensation reaction of melamine and cyanuric chloride in the presence of N,N‐dimethylmethanamide as a high boiling point nonnucleophilic base. Then composite films of PANI/g‐C₃N₄ were prepared by in situ electrochemical polymerization of an aniline solution containing g‐C₃N₄. Different concentrations of g‐C₃N₄ were utilized to improve the electrochemical performances of the hybrids. The resulting PANI/g‐C₃N₄ composite films were characterized by X‐ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and ultraviolet–visible diffuse reflection spectroscopy techniques. The electrochemical performance of the composites was evaluated by cyclic voltammetry (CV). Application of the prepared samples has been evaluated as supercapacitor material in 0.5 M H₂SO₄ solution using CV technique. The specific capacitances of PANI/g‐C₃N₄ composite films were higher than obtained for pure PANI films. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44059.     

Fluorescence turn‐on chemical sensor based on water‐soluble conjugated polymer/single‐walled carbon nanotube composite

A chemical sensor for methyl viologen (MV²⁺), based on a water‐soluble conjugated polymer/single‐walled carbon‐nanotube (SWNT) composite, was fabricated. Water‐soluble poly(m‐phenylene ethynylene) with sulfonic acid side‐chain groups (mPPE‐SO₃) was synthesized via a Pd‐catalyzed Sonogashira coupling reaction and used to prepare a highly stable mPPE‐SO₃/SWNT composite with strong π–π interactions in water. The relationship between the optical properties and sensing capability of the mPPE‐SO₃/SWNT composite in aqueous solution was investigated. The addition of MV²⁺ enhanced the fluorescence intensity of the mPPE‐SO₃/SWNT composite by inducing a conformational change of the polymer from a helical to a random‐coil structure. The water‐soluble mPPE‐SO₃/SWNT composite enabled highly sensitive fluorescence detection of MV²⁺ in aqueous solutions with no precipitation resulting from reaggregation of the SWNTs. This mPPE‐SO₃/SWNT composite sensor system is therefore an effective turn‐on chemical sensor for MV²⁺. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43301.     

A New Class of 3′‐Sulfonyl BINAPHOS Ligands: Modulation of Activity and Selectivity in Asymmetric Palladium‐Catalysed Hydrophosphorylation of Styrene

Palladium‐catalysed monophosphorylation of (R)‐2,2′‐bisperfluoroalkanesulfonates of BINOL (R^F=CF₃ or C₄F₉) by a diaryl phosphinate [Ar₂P(O)H] followed by phosphine oxide reduction (Cl₃SiH) then lithium diisopropylamide‐mediated anionic thia‐Fries rearrangement furnishes enantiomerically‐pure (R)‐2′‐diarylphosphino‐2′‐hydroxy‐3′‐perfluoralkanesulfonyl‐1,1′‐binaphthalenes [(R)‐ 8ab and (R)‐ 8g–j ], which can be further diversified by Grignard reagent (RMgX)‐mediated CF₃‐displacement [→(R)‐ 8c–f ]. Coupling of (R)‐ 8a–j with (S)‐1,1′‐binaphthalene‐2,2′‐dioxychlorophosphine (S)‐ 9 generates 3′‐sulfonyl BINAPHOS ligands (R,S)‐ 10a–j in good yields (43–82%). These new ligands are of utlility in the asymmetric hydrophosphonylation of styrene ( 1 ) by 4,4,5,5‐tetramethyl‐1,3,2‐dioxaphospholane 2‐oxide ( 2 ), for which a combination of the chiral ligands with either [Pd(Cp)(allyl)] or [Pd(allyl)(MeCN)₂]⁺/NaCH(CO₂Me)₂ proves to be a convenient and active pre‐catalyst system. A combination of an electron‐rich phosphine moiety and an electron‐deficient 3′‐sulfone moiety provides the best enantioselectivity to date for this process, affording the branched 2‐phenethenephosphonate, (−)‐iso‐ 3 , in up to 74% ee with ligand (R,S)‐ 10i , where Ar=p‐anisyl and the 3′‐SO₂R group is triflone.     

Systematic synthesis of (Gd1−xLax)2O2SO4:Tb3+ and (Gd1−xLax)2O2S:Tb3+ nanophosphors for remarkably enhanced luminescence

Coprecipitation with rare-earth nitrate, ammonium sulfate, and ammonium hydroxide produced hydroxide-type amorphous precursors incorporating sulfate and carbonate anions, from which [(Gd_1−xLa_x)_0.99Tb_0.01]₂O₂SO₄ and [(Gd_1−xLa_x)_0.99Tb_0.01]₂O₂S (x = 0, 0.15, 0.3, 0.5, 0.65, 0.8, and 1) were obtained as two series of nanophosphors by calcination at 950°C in air and hydrogen, respectively. The detailed characterization by X-ray diffractometer, scanning electron microscopy/transmission electron microscopy, Brunauer–Emmett–Teller, and particle sizing confirmed that solid solutions were directly formed and that the products have small crystallite size, unimodal size distribution, and high specific surface area, revealing the advantages of the synthesis method. Photoluminescence study revealed that La³⁺ admixture may significantly improve the 545 nm main emission of Tb³⁺ for both the phosphor series. Furthermore, the 545 nm main emission of [(Gd_1−xLa_x)_0.99Tb_0.01]₂O₂SO₄ was identified to have an excellent thermal stability, which retained over 90% of its room-temperature intensity at 150°C (no quenching for Gd₂O₂SO₄:Tb³⁺). The two series of phosphors were comparatively studied for their excitation and luminescence performances, as a function of temperature and La³⁺ content, and the results were rationalized by considering bandgap, crystal structure, UV absorption, and the character of chemical bonds.