Sulfamic Acid Research Articles

Sulfamic acid market to generate $238 bn, at 4.6% CAGR by 2031

Sulfamic acid market to generate $238 bn, at 4.6% CAGR by 2031

Sulfamic acid modified UiO-66 metal-organic framework for biodiesel production: Process optimization using response surface methodology, kinetics, and thermodynamic study

A novel sulfamic acid-modified UiO-66 metal–organic framework (UiO-66/SA) catalyst was synthesized in this work for the esterification of oleic acid to biodiesel. Oleic acid was used as a test substrate as it constitutes a major proportion of several biodiesel feedstocks like Jatropha curcas oil, karanja oil, and waste cooking oil. The catalyst was extensively characterized by XRD, TGA, FT-IR, BET, SEM, CHNS and XPS. The catalyst demonstrated a high acidity of 1.4 mmol g−1 evaluated by ammonia-temperature programmed desorption (NH3-TPD) analysis. Central composite design (CCD) approach of response surface methodology (RSM) was used to process the optimization of various parameters (RSM) where, a maximum biodiesel yield of 94.4 ± 0.3 % was obtained under the optimized reaction conditions of methanol to oil molar ratio of 21.9:1, catalyst loading of 7.6 wt%, reaction temperature of 85 °C, and reaction time of 1.8 h. The activation energy for the esterification reaction was found to be 41.56 kJ mol−1 and further, the thermodynamic study confirmed the endothermic nature of the reaction. Multiple regressions and analysis of variance (ANOVA)were used to fit the experimental data to a quadratic equation.

Production of Zn-Ti alloy electrodeposition for biomedical applications

Acidic sulphate bath having ZnSO4, TiSO4 and sulphamic acid, was optimized for the deposition of bright Zn-Ti coating on mild steel. The effect of current density, on deposit characters, such as corrosion rate, thickness, and hardness were discussed. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) methods were used to evaluate the corrosion properties of the deposit. The composition of deposits was determined by energy dispersive X-ray (EDX) analysis. Scanning electron microscopy (SEM) was used to examine the surface topography of the deposited layer. Atomic force microscopy (AFM) was used to determine the surface roughness. A new and low-priced sulphate bath, for bright Zn-Ti coatings on mild steel has been proposed, and the results indicate better corrosion resistance properties, and these coatings can be used for biomedical tools like Tuning fork, etc, applications.

SULFATION OF BIRCH WOOD XYLAN WITH SULFAMIC ACID IN THE PRESENCE OF ACTIVATORS: EXPERIMENT AND THEORY

Xylan is a polysaccharide found in plant cell walls. It is considered to be a biodegradable polymer, which does not affect negatively the environment. Sulfated xylan derivatives exhibit valuable bioactive properties, in particular, anticoagulant and hypolipidemic. We report on the development of a new method for sulfation of birch wood xylan. Activators of the sulfation reaction with sulfamic acid have been evaluated. Numerical methods have been used to establish the optimum process parameters that ensure the maximum sulfur content in the reaction product. The incorporation of a sulfate group has been confirmed by infrared and nuclear magnetic resonance spectroscopy, and elemental analysis. The initial and sulfated xylans have been comprehensively studied by theoretical methods and the most favorable conformations of the initial xylan and its sulfate have been established.

Corrosion Prevention of Copper in 2.0 M Sulfamic Acid Using Novel Plant Extract: Chemical, Electrochemical, and Theoretical Studies.

Copper corrosion was suppressed when a lupine extract was immersed in a 2 M sulfamic acid (H2NSO3H) solution. Numerous methods, including mass loss (ML), dynamic potential polarization (PL), and electrochemical impedance (EIS), were employed in these experiments, in addition to theoretical computations such as density functional theory (DFT), Fukui function, and Monte Carlo simulations. Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM) were used to analyze the Cu surface's composition and determine its form. Mass loss (ML) was used to examine the inhibition rate of copper corrosion in sulfamic acid at 25 °C in the presence of lupine extract. After examining how it behaved throughout the adsorption process on copper, it was discovered that it follows the Langmuir isotherm and chemical adsorption. An analysis of the PL curves indicates that the lupine extract is a mixed-type inhibitor. It was shown that the inhibitory efficiency increased to 84.2% with increasing lupine concentration. Additionally, as the data show, the efficiency of inhibitors is diminished by increasing temperatures. Theoretical calculations and experimental data were compared using Monte Carlo simulation (MC) and density functional theory (DFT).

Crystal growth, structural, vibrational, spectroscopic studies of novelly synthesized NLO active melaminium sulfamate single crystal: Experimental and theoretical approach

Semi-organic nonlinear optical (NLO) melaminium sulfamate (MASA) single crystals were synthesized by slow evaporation method and analyzed by using X-ray diffraction, UV–vis, FT-IR and FT-Raman experiments. Single crystal X-ray diffraction (SXRD) analysis confirms that MASA crystal belongs to triclinic system with centrosymmetric space group P-1. The quantum chemical calculation were carried out using density functional theory (DFT) with B3LYP/6-31+G(d) basis set. The intermolecular interactions were deeply analyzed by NBO analysis. The molecule with intermolecular N-H⋯N and N-H⋯O hydrogen bonds show notable vibrational effect. The optical property of MASA was evaluated by UV–vis optical transmittance spectrum. Thermal stability of the grown crystal was performed by using TG-DTA analysis. The frontier molecular orbital analysis illustrates the charge transferred from sulfamate anion to melaminium cation. Hirshfeld and 2D fingerprint plot reveals the intermolecular N-H⋯O and N-H⋯N contacts of MASA molecule. The existence of various functional groups and vibrational modes are affirmed by Fourier transform infrared (FT-IR) and FT-Raman spectral analysis. Additionally, the molecular electrostatic potential (MESP) and topological analysis such as electron localization function (ELF), reduced density gradient(RDG), localized orbital locator(LOL) and atoms in molecule(AIM) have been used to predict the intermolecular interaction, especially the hydrogen bonds. The hydrogen atom from sulphamic acid was transferred to the melamine molecule giving the singly protonated melaminium cation. The outcome of SXRD, UV–visible, TG/DTA, HOMO–LUMO, NLO and Z-Scan values were compared with earlier reported compounds and amongst the analyzed compound MASA shows good NLO activity. The NLO activity of MASA was analyzed theoretically and experimentally by DFT and Z-scan method.

Synthesis, Computational and Antimicrobial Study of 2-(2-Hydrazinyl)thiazole Derivatives

In the present investigation, we report a combined computational and experimental study of eight thiazole derivatives (4a-4h) obtained from 3,4-dihydronaphthalen-1(2H)-one. A green chemistry protocol comprising PEG-400 and sulfamic acid was employed for the synthesis of eight diverse thiazole derivatives from 3,4-dihydronaphthalen-1(2H)-one, thiosemicarbazide and various phenacyl bromides. The synthetic strategy provides benefits like short reaction time, high yield, and non-chromatographic purification. The compounds were structurally confirmed on the basis of IR, 1HNMR and 13C NMR. The obtained thiazole derivatives were studied using the density functional theory (DFT) method employing B3LYP/6-311G(d,p) level of theory for optimization and Time-Dependent DFT (TD-DFT) approach for examining electronic energies and UV-Vis characteristics. Various computational parameters like bond length, bond angles, HOMO, LUMO, MESP, Mulliken charges, and global descriptors are obtained and discussed. The UV-Vis study the in gas phase and DMSO solvent was investigated to obtain various insights such as absorption energies oscillator strength, configurations and transitions of examined thiazole derivatives. The effect of polar solvent has augmented the absorption wavelength of all studied thiazole derivatives. The experimental and simulated UV-Vis data correlate with each other prompting the effectiveness of the computed method. The scaled and experimental wavenumbers provided the appropriate assignment of various vibrational signals. The antibacterial study was performed against E. coli, P. aeruginosa, and S. aureus which demonstrated the strong antibacterial potential against S. aureus. The antifungal study against C. albicans revealed that these compounds are poor antifungal agents. The DPPH and OH radical assays were used to establish the % radical scavenger effects and results showed that these derivatives are good antioxidant agents. The % hemolytic activity of the tested compounds showed that all compounds fall within the acceptable toxicity limit. Importantly in slico ADME and toxicity prediction studies of these compounds highlighted good ADME profile with no hepatotoxicity, immunotoxicity and cytotoxicity.

Simple and Rapid Voltammetric Method Using a Gold Microwire Electrode to Measure Inorganic Arsenic in Holopelagic Sargassum (Fucales, Phaeophyceae)

The valorization of massive strandings of holopelagic Sargassum spp. is strongly limited by high levels of inorganic arsenic (Asi) that are potentially above the limit of current regulations. Monitoring Asi in algal biomass is currently achieved using standard chromatographic separation followed by spectroscopic detection. Here, we propose an alternative simpler procedure based on the extraction of Asi from the freeze-dried algal powder in deionized water and the electroanalytical detection of the diluted extract at a gold-microwire electrode. The protocol was optimized both in terms of extraction (powder/water ratio, extraction time, temperature) and electrolyte used for the voltammetric detection. Two electrolytes were tested: one composed of citric acid, sulfamic acid and KCl (pH 2.0) and another composed of an acetate buffer (pH 4.7) and NaCl. We demonstrate here that Asi determination is possible with the first electrolyte but it is necessary to deal with a relative unstable signal. Measurement of Asi was best achieved with the second electrolyte (acetate buffer and NaCl) with the following optimized electrochemical conditions: deposition potential of −1.2 V, deposition time of 30 seconds and linear scan voltammetry. Voltammetric results were then compared to a reference method (HPLC-ICP-MS) using different morphotypes of holopelagic Sargassum spp. (S. natans VIII, S. natans I and S. fluitans III), using commercial extracts of brown seaweeds and using a Hijiki certified reference material. Very good agreement was obtained between our novel method and HPLC-ICP-MS. Both methods show that inorganic arsenic is almost entirely present as As(V) in Sargassum spp. extracts.

An ultraviolet shielding material based on lignin nanoparticles engineered with deep eutectic solvents for long-term outdoor application

Ultraviolet radiation (UV) has a significant effect on the wood, and the commonly used UV shielding agents are easily degraded. Lignin is a bio-based UV screening agent and tuning of its nanoparticles is meaningful for realizing the UV shielding properties and stability of composites. With the modification of the deep eutectic solvents based on sulfamic acid and urea, lignin nanoparticles with amino functional groups were prepared, and a protective layer with UV shielding properties was constructed on the surface of the poplar veneer. The phenolic hydroxyl groups, carbonyl groups, and conjugated structure of lignin nanoparticles endowed the composites with the properties of UV shielding, photothermal conversion, and photothermal de-icing. The results of this study provide a benchmark for realizing the low-cost and sustainable preparation of wood composites with UV shielding and are conducive to promoting the high-value application of lignin nanoparticles.

Hydrazine Sulfonic Acid, NH3 NH(SO3 ), the Bigger Sibling of Sulfamic Acid.

The reaction of hydrazine hydrate, N2 H4 ⋅ H2 O, and SO3 leads to hydrazine sulfonic acid (Pca21 , a=849.59(4) pm, b=482.18(2) pm, c=832.17(4) pm). Structure elucidation reveals the zwitter-anionic nature of the compound according to NH3 NH(SO3 ). With the barium salt Ba[NH2 NH(SO3 )]2 (H2 O), a first salt of hydrazine sulfonic acid has been prepared (P , a=489.75(5) pm, b=737.52(7) pm, c=1317.4(1) pm, α=88.238(4)°, β=84.761(4)°, γ=79.701(4)°). The compounds were characterized by vibrational spectroscopy, DFT calculations and thermal analyses.

A novel approach to determine residual aldehyde content in conjugated polysaccharides with 3-methyl-2-benzothiazolinonehydrazon (MBTH) by colorimetric method, automation, and HP-SEC

Polysaccharide activation by periodate oxidation to form aldehydes, followed by conjugation with proteins via reductive amination is a general procedure to make polysaccharide-protein conjugate vaccines. Controlling the level of residue aldehyde content after conjugation is critical to ensure vaccine product stability. Herein, to support conjugation process optimization, we developed a 3-methyl-2-benzothiazolone hydrazone (MBTH) chemistry-based colorimetric method, which can measure low-level residual aldehyde polysaccharide-protein conjugate in high throughput 96-well plate format. This mechanism of detection works in two steps. First, MBTH reacts with the aldehyde group to form azine. Then the excess MBTH was oxidized by ferric ammonium sulfate in sulfamic acid to form a reactive cation, which reacts further with azine to form formazan, a characteristic blue chromophore at 610 nm, for colorimetric detection. The method performance, including detection limit, linearity range, matrix effect, kinetics, and color stability was systematically studied. For samples with severe matrix interference, a supplemental size exclusion chromatography (SEC) method was also developed as an alternative method.

Sulfamic Acid Supported Zr-MOF: An Effective Catalyst for One-Step Synthesis of Novel 6-Amino-5-(4-Amino-2-Oxo-2H-Chromen) Analogs

Sulfamic acid-functionalized Zr-MOF-NH2 was used as an active acidic metal-organic framework catalyst for the synthesis of new 6-amino-5-(4-amino-2-oxo-2H-chromen) (AAOC) analogs via a one-step reaction between 2-hydroxy-5-(aryldiazenyl)benzaldehyde, 4-aminocumarin, and 6-amino-1,3-dimethyluracil or 6-amino-uracil in EtOH under reflux conditions. The resulting UiO-66-NHSO3H was characterized by employing different types of spectroscopic techniques such as XRD, BET, FESEM, EDS, FT-IR, and TGA. In addition, ease of procedure, short reaction time, and recycling of the catalyst without much change in the catalytic activity are the advantages of this method.

Influence of Sm doping on the optical, mechanical, electrical, thermal and z-scan analysis of sulphamic acid single crystal for nonlinear optical device applications

Influence of Sm doping on the optical, mechanical, electrical, thermal and z-scan analysis of sulphamic acid single crystal for nonlinear optical device applications

Catalytic liquefaction of starch by sulfamic acid and its curing kinetics for preparing polyurethane

Catalytic liquefaction of starch by sulfamic acid and its curing kinetics for preparing polyurethane

Fabrication of magnesium oxide–calcium alginate hydrogel for scaffolding yttrium and neodymium from aqueous solutions

In this research, the possibility of using sustainable nano-MgO/Ca-alginate beads for efficient sorption of some rare earth metal ions such as neodymium(III) and yttrium(III) from an aqueous acidic solution was explored. The nano-MgO/Ca-alginate beads adsorbent was characterized before and after sorption of Nd(III) and Y(III) using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), energy dispersive X-ray analysis (EDX), and X-ray diffraction (XRD) techniques. Batch sorption parameters were investigated, such as contact time, initial metal ion concentration, and adsorbent dose (V/m). The calculated experimental results showed that the suitable selected sorption conditions were carried out using 100 mg/L of Nd(III) and Y(III) with nano MgO/Ca-alginate beads (contact time = 90 min, pH = 2, V/m = 0.05 L/g). The maximum sorption capacity of 0.1 g of nano MgO/Ca-alginate was found to be 7.85 mg/g and 5.60 mg/g for Nd(III) and Y(III), respectively. The desorption of Nd(III) and Y(III) from the loaded nano MgO/Ca-alginate was achieved with 1.0 M sulfamic acid and found to be 51.0% and 44.2%, respectively. The calculated thermodynamic parameters for the nano MgO/Ca-alginate/Nd/Y system show that the positive charge of ΔHo confirmed the endothermic nature of the sorption process, ΔSo (positive) indicates an increase in reaction system disordering, and ΔGo (negative) indicates a spontaneous process. These kinetic results indicate that the sorption process of Nd(III) and Y(III) on nano MgO/Ca-alginate beads is performed by the chemisorption process.

Sulfamic acid functionalized PVC: a remarkably efficient heterogeneous reusable catalyst for the acid-catalyzed reactions

Sulfamic acid functionalized PVC: a remarkably efficient heterogeneous reusable catalyst for the acid-catalyzed reactions

Synthesis of Birch Wood Xylan Sulfate in the Sulfamic Acid–Urea Melt

AbstractThe synthesis of polysaccharide sulfates without harmful solvents used is a serious environmental problem. A method for the synthesis of xylan sulfate using the sulfamic acid–urea melt as a sulfating agent without solvents is proposed. The melt is prepared by heating the sulfamic acid–urea mixture with a molar ratio of 1 : 1 at a temperature of 110 °C. This ratio allows significant reduction of side reactions, in particular, carbamation of xylan. Sulfation is carried out at temperatures of 110,115, 120, 125, and 130 °C. The maximum yield and degree of substitution (DSsulfate 1.40) are attained at atemperature of 115 °C. The proposed method makes it possible to synthesize xylan sulfate rapidly (for 0.5 h) and without contamination of the obtained product with toxic solvents, e. g., dimethyl sulfoxide, pyridine, etc. The composition and structure of initial and sulfated xylan are confirmed by FTIR, NMR, GC, and elemental analysis.

The mechanism of self-assembly of lignin in deep eutectic solvent based on sulfamic acid and urea through molecular dynamics simulation

Due to the diversity of industrial lignin sources and the complexity of its structure, its application as a high-value material is limited. Lignin nanoparticles (LNPs) have emerged as a hotspot for research due to their advantages of high specific surface area and high dispersion and the solvent transfer method is commonly used for the preparation of LNPs. In this paper, LNPs were prepared by solvent transfer method using DES based on sulfamic acid and urea (S/U DES) as solvent and water as anti-solvent. To explore the internal mechanism of the self-assembly of nanoparticles, a theoretical model of the solvent system and model lignin compound was constructed with the assistance of quantum chemistry and molecular dynamics theories. Through classical molecular dynamics (MD) simulations, the interaction energy, radius of gyration (ROG), solvent accessible surface area (SASS), radial and spatial distribution function (RDFs/SDFs), hydrogen bonding, and the morphology changes were analyzed to reveal the internal mechanism of self-assembly of model lignin compounds in S/U DES. This study is useful in revealing the mechanism of interaction between lignin and DES, as well as providing a benchmark for the green and efficient preparation of lignin nanoparticles.

Failure analysis and quick recovery of a low‐temperature distillation station

AbstractA coupling model based on hazard and operability analysis (HAZOP) and fault tree analysis is proposed and used to analyze the failure of a low‐temperature distillation station (LTDS). It is found that the formation of scale in the deamination tower in the LTDS is the most significant cause for the failure. The scale was mainly composed of SrSO4, CaCO₃, CaSO4, and MgCO₃, which were determined by various techniques from the gas‐field water. Dynamic weight loss experiments were conducted to estimate the corrosion rate of 304 steel with different cleaning solutions. The corrosion behaviors of the metal in the deamination tower were further investigated in three types of cleaning solution via potentiodynamic polarization method. The cleaning solution composed of 6% sulfamic acid, LAN826, JFC, and a defoaming agent could safely and quickly remove the scale covering the LTDS at 50°C. In addition, the optimal cleaning time was found to be 6 h.

Back Cover: Superprotonic Conductivity of MOFs Confining Zwitterionic Sulfamic Acid as Proton Source and Conducting Medium (Angew. Chem. Int. Ed. 29/2023)

Superprotonic conductivity, utilizing MOFs embedded with a moderately acidic guest—zwitterionic sulfamic acid (HSA)—was demonstrated by Myoung Soo Lah et al. in their Research Article (e202302376). HSA not only acted as a proton source, but also as a proton-conducting medium. The MOFs, which had been filled with high quantities of HSA using a sustained concentration gradient method, exhibited impressive superprotonic conductivity, in the order of 10−1 S cm−1. Furthermore, they maintained their stability for a period of 7 days.