Sulfamic Acid Research Articles

A simple preparation process for an efficient nano-formulation: small molecule self-assembly based on spinosad and sulfamic acid

The abuse of toxic organic solvents and surfactants has caused immeasurable damage to human health and the environment.

Sulfamic acid catalyzed oxonium-ene reactions under ball milling conditions: Straightforward access to highly functionalized Oxabicyclo[3.2.1]octenes

Herein, we report a facile green procedure for the synthesis of oxabicyclo[3.2.1]octenes using sulfamic acid as catalyst under solvent-free ball milling conditions. A series of aldehydes or epoxides underwent oxonium-ene reaction with (−)-terpinen-4-ol under optimized conditions to produce a variety of oxabicyclo[3.2.1]octene derivatives. The excellent selectivity, higher isolated yields of the products, use of mild catalyst and solvent-free ball milling conditions, and recyclability are the major advantages of the present procedure.

Anhydrous proton conductivity of electrospun phosphoric acid-doped PVP-PVDF nanofibers and composite membranes containing MOF fillers.

A high-temperature proton exchange membrane was fabricated based on polyvinylidene fluoride (PVDF) and polyvinylpyrrolidone (PVP) blend polymer nanofibers. Using electrospinning method, abundant small ionic clusters can be formed and agglomerated on membrane surface, which would facilitate the proton conductivity. To further enhance the conductivity, phosphoric acid (PA) retention as well as mechanical strength, sulfamic acid (SA)-doped metal–organic framework MIL-101 was incorporated into PVP-PVDF blend nanofiber membranes. As a result, the anhydrous proton conductivity of the composite SA/MIL101@PVP-PVDF membrane reached 0.237 S cm−1 at 160 °C at a moderate acid doping level (ADL) of 12.7. The construction of long-range conducting network by electrospinning method combined with hot-pressing and the synergistic effect between PVP-PVDF, SA/MIL-101 and PA all contribute to the proton conducting behaviors of this composite membrane.

Особенности свойств сульфаминовой кислоты, повышающие эффективность кислотных обработок

Особенности свойств сульфаминовой кислоты, повышающие эффективность кислотных обработок

Corrosion behavior of additive manufactured Ti-6Al-4V in sulfamic acid cleaning solution

The specific microstructural features and phase composition lead to different corrosion behaviors of SPS and additive manufactured Ti-6Al-4V alloys.

Fabrication of sulfamic acid functionalized magnetic nanoparticles with denderimeric linkers and its application for microextraction purposes, one-pot preparation of pyrans pigments and removal of malachite green

Abstarct In this research, we stated the fabrication of an innovative sulfamic acid functionalized magnetic nanoparticles (Fe3O4@PAMAM-SO3H) with denderimeric linkers. FT-IR, TEM, XRD, FE-SEM, and TGA methods were carried out to characterize the catalyst. Eventually, The catalytic prowess of the Fe3O4@PAMAM-SO3H was tested to synthesize highly substituted pyrans. The obtained magnetic sorbent was also used to remove malachite green (MG) and magnetic solid phase extraction of bisphenol A (BPA) as an organic pollutant from aquoues media in the form of magnetic solid-phase extraction (MSPE) method. The maximum adsorption capacity (qm) of the prepared sorbent for MG found by the Langmuir isotherm was 1250 mg g−1 at 333.15 K. In addition, the MSPE of BPA was carried out and high performance liquid chromatography (HPLC) was employed to quantify the extracted analyte. The method presented a linearity range of 0.2–200 µg L−1. The obtained relative standard deviations (RSDs) were lower than 7.1%. The limit of quantification (LOQ) and limit of detection (LOD) were also calculated to be 0.18 and 0.05 µg L−1, respectively. Relative recoveries higher than 97.5% were attained for analysis of various selected real samples.

Ultrasonically-mediated one-pot synthesis of substituted imidazoles via sulfamic acid functionalized hollow magnetically retrievable solid-acid catalyst

In this work, we report the synthesis of functionalized hollow magnetite spheres (HMS) which were synthesized through gas-bubble assisted Ostwald ripening approach and post-functionalized with sulfamic acid groups. The fabricated material was used as an efficient solid-acid catalyst for one-pot three-component synthesis of medicinally important tri-substituted imidazoles under ultrasonic irradiation. Some of the striking features of the present protocol over existing routes are environmentally benign synthesis, milder reaction conditions, excellent yields, high selectivity, short reaction times, use of ultrasound as green energy source, less waste generation and effortless magnetic recovery and recycling of the catalyst. Further, the synthesized magnetite spheres extend the scope of ‘double functionalization’, i.e., the acidic groups can be immobilized on both internal and external surfaces which provides high acid loading as compared to previously reported solid supports.

A nano-sensing composite platform combining magnetic and emissive features: Fabrication and performance

The following paper was devoted to two nitrite sensing platforms having a core-shell structure, where Fe3O4 nanoparticles were used as core, a silica molecular sieve MCM-41 was constructed as shell and two rhodamine chemosensors were synthesized as probe, respectively. This magnetic core endowed these two sensing platforms with site-specific aggregation ability. They were carefully characterized through their electron microscopy images, porous analysis, magnetic performance, IR curves and thermal stability analysis. Experimental result suggested that these two sensing platforms were sensitive towards nitrite and their emission was quenchable by nitrite. A static sensing mechanism between probe and analyte through an additive reaction was established by emission decay lifetime analysis. These two sensing platforms showed limit of detection as low as 1.2 μM. Additionally, after their nitrite sensing, these two sensing platforms and their emission could be recovered by sulphamic acid, realizing recyclability.

A technique for uranium and plutonium determination using coulometric potentiostatic facility UPK-19 for analysis of mixed-oxide fuel

The content of uranium and plutonium is the main characteristic of mixed uranium-plutonium oxide fuel, which is strictly controlled and has a very narrow range of the permissible values. We focused on developing a technique for measuring mass fractions of uranium and plutonium by controlled potential coulometry using a coulometric unit UPK-19 in set with a R-40Kh potentiostat-galvanostat. Under conditions of sealed enclosures, a special design of the support stand which minimized the effect of fluctuations in ambient conditions on the signal stability was developed. Optimal conditions for coulometric determination of plutonium and uranium mass fractions were specified. The sulfuric acid solution with a molar concentration of 0.5 mol/dm3 was used as a medium. Lead ions were introduced into the background electrolyte to decrease the minimum voltage of hydrogen reduction to –190 mV. The addition of aluminum nitride reduced the effect of fluoride ions participating as a catalyst in dissolving MOX fuel samples, and the interfering effect of nitrite ions was eliminated by introducing a sulfamic acid solution into the cell. The total content of uranium and plutonium was determined by evaluation of the amount of electricity consumed at the stage of uranium and plutonium co-oxidation. Plutonium content was measured at the potentials, at which uranium remains in the stable state, which makes it possible to subtract the contribution of plutonium oxidation current from the total oxidation current. The error characteristics of the developed measurement technique were evaluated using the standard sample method and the real MOX fuel pellets. The error limits match the requirements set out in the specifications for MOX fuel. The technique for measuring mass fractions of uranium and plutonium in uranium-plutonium oxide nuclear fuel was certified. The relative measurement error of the mass fraction of plutonium and uranium was ±0.0070 and ±0.0095, respectively. The relative error of the ratio of the plutonium mass fraction to the sum of mass fractions of uranium and plutonium was ±0.0085.

Sulfamic: acid incorporated tin oxide: Acidity and activity relationship

Herein we study the activity and acidity relationship, Sulfamic acid (SA) has been incorporated with tin oxide (Sn). Acidity measurement confirmed the presence of dual-acidic sites. SA hinders the crystallization and inhibits SnO2 crystal growth. The particle size of SnO2 (2.1–8.2 nm) and the SBET values of samples were found to be dependent on the SA content and calcination temperatures. The increase in the surface acidity was found to occur with increasing the thermal treatment up to 450 °C, while further increasing of calcination temperature is accompanied by a decrease in the surface acidity. Lewis and Bronsted acid sites play important role in the catalytic activity, The SA-Sn nanoparticles are efficient for the synthesis of 14-aryl-14H-dibenzo[a,j] xanthene under solvent-free conditions in good to excellent yields and the sample contains 25 wt% SA has the highest activity than the others under the same reaction conditions.

Sulfated Derivatives of Arabinogalactan and Their Anticoagulant Activity

A comparison of IR spectra and molecular weight distribution of arabinogalactan sulfates as sodium and ammonium salts obtained using various sulfating reagents was performed. According to the data, sulfated derivatives of arabinogalactan differ from each other in the nature of hydrogen bonds and molecular weight distribution. Using coagulological tests during activation of coagulation of platelet-poor human plasma in vitro, the anticoagulant properties of sulfated arabinogalactan derivatives in various salt forms differing in the preparation method, sulfation degree, and molecular weight were studied. It was found that the sample in the form of the sodium salt of sulfated arabinogalactan (SAG 1) with a sulfur content of 13.2 wt % and a polydispersity degree of 1.52 exhibited twofold greater anticoagulant activity than the sample in the form of the ammonium salt of sulfated arabinogalactan (SAG 2) with a sulfur content of 6.6 wt % and a polydispersity degree of 1.30. The antithrombin (aIIa) activity of the samples obtained by sulfation with a complex of pyridine and sulfuric anhydride (SAG 1) and a complex of sulfamic acid (SAG 2) was 23.42 ± 1.86 and 10.20 ± 1.50 U/mg, respectively; the value of the antifactor Xa activity of SAG 1 and SAG 2 was 2.13 ± 0.42 and 0.37 ± 0.08 U/mg; the aIIa/aXa ratio for SAG 1 and SAG 2 was 11 and 28, respectively. The antifactor Xa (aXa) activity of SAG, which is lower than that of unfractionated heparin (UFH), and a high aIIa/aXa activity ratio may contribute to less provocation of bleeding by SAG samples compared to UFH.

Synthesis, crystal structure, Hirshfeld surface analysis, biological evaluation, DFT calculations, and in silico ADME analysis of 4-arylidene pyrazolone derivatives as promising antibacterial agents

The present paper describes an ultrasound-assisted synthesis of a series of 4-arylidene-1H-pyrazol-5(4H)-one derivatives (3a-i) catalyzed by sulfamic acid. The prepared compounds were characterized by physical and spectroscopic techniques and for compound 3i by single crystal X-ray diffraction analysis. Theoretical calculations such as molecular structure optimization, frontier molecular orbitals, molecular electrostatic potential, and molecular descriptors have been performed in order to get insight into the molecular structure and chemical reactivity of the synthesized compounds. The antibacterial activity of all compounds was assessed against six bacterial strains, and it was found that these compounds are good inhibitors of Gram-positive bacteria rather than Gram-negative. In addition, good oral bioavailability was predicted for all compounds by in silico calculations of ADME (absorption, distribution, metabolism, and elimination) and pharmacokinetic parameters.

Optimization of starch sulfation process with a deep eutectic solvent-mixture of sulfamic acid:urea

The process of sulphation of potato starch with a deep eutectic solvent, a mixture of sulfamic acid: urea, was optimized. The influence of varying factors was established - the ratio of sulfamic acid: urea (SAA: U), the ratio of starch: sulfating complex (St: SC) and the duration of the process on the sulfur content (wt.%) in the obtained starch sulfate. The data of analysis of variance for the obtained mathematical models indicate good prognostic properties. The optimal conditions for starch sulfation, which provide water-soluble sulfated starch with a high (up to 11.2% wt.) sulfur content, have been established. The optimal conditions for the process of sulfation of potato starch are the ratio SAA: U 1: 2.0-1: 2.2, the ratio St: SC 1: 3.5-1: 4.0 and the duration of the process is 118-120 minutes.

Effect Of Inorganic Components Of Fire Foaming Agents On The Aquatic Environment

Impact on the aquatic medium of the number of inorganic additives that are part of the foaming agents for firefighting is considered in paper. The influence of the most widespread inorganic components on aquatic organisms is analyzed. Significant variability of data is noted. It is proved that the magnesium and sodium chlorides are the safest for the environment and the most dangerous ones are aluminum compounds and sulfamic acid. Inorganic additives based on aluminum, sulfamic acid and sodium bicarbonate are the most dangerous for aquatic living organisms, in the short and long term, and the safest compounds are magnesium and sodium chlorides

Synthesis, Characterization, and In Silico Studies of Novel Spirooxindole Derivatives as Ecto-5'-Nucleotidase Inhibitors.

Ecto-5'-nucleotidase (ecto-5'-NT, CD73) inhibitors are promising drug candidates for cancer therapy. Traditional efforts used to inhibit the ecto-5'-nucleotidase have involved antibody therapy or development of small molecule inhibitors that can mimic the acidic and ionizable structure of adenosine 5'-monophosphate (AMP). Herein, we report an efficient, environment friendly route for the synthesis of non-nucleotide based small molecules, i.e., substituted spirooxindole derivatives 9a-9l and investigated their inhibitory potential on human and rat recombinant ecto-5'-nucleotidase isozymes. These attempts have resulted in the identification of compound 9f (IC50 = 0.15 ± 0.02 μM) inhibitor on h-ecto-5'-NT which showed 280-fold higher inhibition and compound 9h (IC50 ± 0.19 ± 0.03 μM) on r-ecto-5'-NT with 406-fold enhanced inhibition than reference standard sulfamic acid. Moreover, in silico studies were carried out to assess binding interactions of potent compounds within enzyme active sites and demonstrated excellent correlation with the experimental findings.

One‐pot multicomponent synthesis of novel 2‐(piperazin‐1‐yl) quinoxaline and benzimidazole derivatives, using a novel sulfamic acid functionalized Fe3O4 MNPs as highly effective nanocatalyst

The immobilization of sulfonic acid on the surface of Fe3O4 magnetic nanoparticles (MNPs) as a novel acid nanocatalyst has been successfully reported. The morphological features, thermal stability, magnetic properties, and other physicochemical properties of the prepared superparamagnetic core–shell (Fe3O4@PFBA–Metformin@SO3H) were thoroughly characterized using Fourier transform infrared (FTIR), X‐ray diffraction (XRD), energy‐dispersive X‐ray spectroscopy (EDS), field‐emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), thermogravimetric analysis–differential thermal analysis (TGA‐DTA), atomic force microscopy (AFM), dynamic light scattering (DLS), Brunauer–Emmett–Teller (BET), and vibrating sample magnetometer (VSM) techniques. It was applied as an efficient and reusable catalyst for the synthesis of 2‐(piperazin‐1‐yl) quinoxaline and benzimidazole derivatives via a one‐pot multiple‐component cascade reaction under green conditions. The results displayed the excellent catalytic activity of Fe3O4@PFBA–metformin@SO3H as an organic–inorganic hybrid nanocatalyst in condensation and multicomponent Mannich‐type reactions. The easy separation, simple workup, excellent stability, and reusability of the nanocatalyst and quantitative yields of products and short reaction time are some outstanding advantages of this protocol.

Crystal growth, optical, thermal, mechanical and third-order nonlinear optical properties of L-lysine hydrochloride-doped sulphamic acid single crystals for optical applications

L-lysine hydrochloride-doped sulphamic acid (SA) crystals have been grown by slow evaporation technique. X-ray diffraction experiments confirmed the orthorhombic structure of SA crystal. The doped crystals have high transmission than the pure SA crystal. TG and DTA studies exhibit the title crystals are thermal stability up to 212 °C (pure), 210 °C (1 mol%) and 207 °C (2 mol%). The enhancement of the hardness value in the doped crystal was confirmed by the hardness test. The etch pit density was measured using chemical etching study. The photosensitivity of the grown crystals is 0.10 (pure), 0.36 (1 mol%) and 0.72 (2 mol%). The laser damage threshold (LDT) analyses show that the L-lysine hydrochloride-doped SA crystals have more LDT value than the pure SA crystal. Third-order NLO susceptibility was found to be 5.004, 5.864 and 6.050 × 10–10 esu for pure and L-lysine hydrochloride-doped (1 and 2 mol %) SA crystals, respectively.

Electrochemical, spectroscopic and theoretical studies for acid corrosion of zinc using glycogen

The objective of the work is to introduce and establish anticorrosion capabilities of a novel biopolymer glycogen (GLY) against sulfamic acid (NH2SO3H) induced corrosion of zinc. The corrosion and inhibition studies were done by electrochemical techniques such as potentiodynamic polarization (PDP) measurements and electrochemical impedance spectroscopy technique (EIS). Conditions were optimized to get maximum inhibition efficiency by varying the concentration of the inhibitor in the temperature range of 303–323 K. Activation and thermodynamic parameters were evaluated and discussed in detail. Suitable adsorption isotherm was proposed to fit the experimental results. Scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and atomic force microscopy (AFM) studies were performed before and after the addition of inhibitor. Adsorption of inhibitor was further confirmed by UV–Visible spectroscopy. Quantum chemical calculations were done to establish the correlation between the structure of the inhibitor and its inhibition efficiency. Energy of HOMO, LUMO, energy gap ∆E, dipole moment (µ) Mullikan charges were calculated. Different theoretical factor descriptors like the hardness (η), and softness (σ) electronegativity (χ), global electrophilicity (ω), nucleophilicity (ε) and fraction of electron transferred (ΔN) were calculated. Inhibition efficiency of glycogen increased with increase in its concentration and with temperature. Maximum efficiency of 72% could be achieved for the addition of 0.05 g L−1 of GLY at 323 K. Results were fitted into Langmuir adsorption iostherm. The surface of the metal turned visibly smoother in the presence of GLY. In addition the EDX studies showed increase in carbon content which re-affirmed the adsorption of GLY on the metal surface. The density functional theory (DFT) based theoretical studies supported the experimental observations.

Sulfamic acid functionalized slag for effective removal of organic dye and toxic metal from the aqueous samples

Surface functionalization of blast furnace slag with sulfamic acid (a zwitterion) was performed for the removal of Cr 3+ and methylene blue dye (MB) from water samples. The slag functionalization process was optimized using Response Surface Methodology Design. Statistical analysis of the parameters that include the sulfamic acid amount (A), reaction time (B), and temperature (C) revealed that (A) increase had a negative effect on the adsorption of both pollutants by the zwitterion slag, whereas (B) and (C) increase presented a positive impact. At the optimum condition of 2 g sulfamic acid amount, 50 min reaction time and 37 °C temperature, the prepared slag showed a removal efficiency of more than 90% for both Cr 3+ and MB. Surface characterization by SEM/EDS, FTIR, XPS and surface area analyser, showed an improvement in surface properties and the incorporation of zwitterionic NH 2 + and S O groups of sulfamic acid. Adsorption isotherm and kinetic studies conducted with the zwitterion slag showed the adsorption process was suited to Freundlich isotherm model and pseudo-second-order kinetic model. The thermodynamic study conducted revealed the spontaneity of the process based on the calculated negative Δ G (Gibb’s free energy) values. The prepared zwitterion slag offered easy regeneration with dilute HCl solution and showed a considerable removal (Cr 3+ : 65% and MB: 80%) for both pollutants even after 3 cycles of usage.

Synthesis, characterization, and thermal behavior of amidosulfonates of transition metals in air and nitrogen atmosphere

The amidosulfonates of Mn2+, Co2+, Ni2+, Cu2+ and Zn2+ were prepared by the direct reaction between the metal carbonate and the amidosulfonic acid with heating and stirring. The compounds were characterized by infrared absorption spectroscopy (IRFT), elemental analysis, thermal analysis (TG and DTA) and X-ray diffraction by the powder method. The absorptions observed in IR spectra are associated with N-H and O-H stretching, as well as symmetrical and asymmetric S-O stretching in the sulfonic group. The compounds present X-ray diffraction pattern with well-defined reflections, showing no evidence of isomorphism. The TG-DTA curves allowed to establish the stoichiometry of compounds as M(NH2SO3)2.xH2O, where M = Mn2+, Co2+, Ni2+, Cu2+ and Zn2+ and x ranging from 1 to 4. Dehydration leads to the formation of stable anhydrous. In all cases the respective sulfates are formed as an intermediate. After consecutive steps of decomposition, the respective oxides were obtained: Mn3O4, CoO, NiO, CuO and ZnO. The TG-DTA curves are characteristic for each sample, with thermal events related to dehydration and ligand decomposition.