SYNTHESIS,CHARACTERIZATION, AND COMPARATIVE STUDY OF PYRIDINE DERIVATIVES AS CORROSION INHIBITORS OF MILD STEEL IN HCl MEDIUM

Radical catalysis has been used to achieve addition of dodecanethiol and mercaptoacetic acid to 4-vinylpyridine (4VP), giving 4-(dodecylthiaethyl)pyridine (DTEP) and 4-pyridylethylthia-acetic acid (PETAA). The purified monoadducts have been characterized using ¹H NMR and ¹³C NMR spectroscopy. Inhibition of the corrosion of mild steel in 1 M HCl by 4VP, DTEP, and PETAA has been investigated at 308 K using weight loss measurements, potentiodynamic polarization, and electrochemical impedance spectroscopy (EIS) methods. The results obtained show that PETAA is the best inhibitor and its inhibition efficiency (E %) increases with the inhibitor concentration, reaching up to 93% for DTEP at 10^?3 M. Potentiodynamic polarization studies clearly revealed that the inhibitors changed the mechanism of hydrogen evolution and that they acted as mixed inhibitors but most effectively in the cathodic range.     

Synthesis,characterisation, and chemical degradation of segmented polyurethanes with butylamine for chemical recycling

Polyurethane elastomers (PU) have been synthesized from polytetramethylene glycol 2000 (PTMG 2000); 4, 4′‐diphenylmethane diisocyanate (MDI) and 1, 4‐butanediol (BD) as chain extender. This synthesis has been done in two steps known as prepolymer methods. The concentration of soft segments and hydrogen attachment in the matrices, have been studied. The results show that the glass transition of the soft segment T_g(s) do not take any changes with the concentration of the soft segment in the matrices. Although, the glass transition temperature of the hard segment T_g(H) increases when the concentration of the hard segment increases in the matrices. In general, the properties of the polyurethane elastomers depend on the extenders nature, the synthesis methods, phase segregation etc. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Piperazine derivatives as inhibitors of the corrosion of mild steel in 3.9 M HCl

The inhibitory action of two piperazine derivatives, 1-benzyl piperazine (P1) and bis(1-benzylpiperazine) thiuram disulfide (P2) on the corrosion of mild steel in 3.9 M HCl at different concentrations has been investigated in the temperature domain 298–333 K. Both weight loss measurements and potentiodynamic polarization methods showed that P2 was the best inhibitor and that its inhibition efficiency increased with concentration to a value >92% at 10⁻³ M. Potentiodynamic polarization studies clearly revealed that P2 acts as cathodic-type inhibitor. The activation energy for the corrosion rates was evaluated in the temperature range 298–333 K. Adsorption of P2 on the mild steel surface in 3.9 M HCl followed a Langmuir isotherm model. A physical adsorption phenomenon is proposed.     

Adsorption properties of Rosmarinus officinalis oil as green corrosion inhibitors on C38 steel in 0.5 M H_2SO_4

Rosmarinus officinalis  essential oil obtained by hydrodistillation was tested as corrosion inhibitor of steel in 0.5~M H₂SO₄ using weight loss measurements, and electrochemical polarisation methods. Results obtained indicate that the corrosion rate is reduced and R.officinalis oil adsorbs on the metal surface and then inhibits corrosion process. Its inhibition efficiency increases with oil increasing content to reach 61 % at 1 g/L. Polarisation curves indicate that RO acts as a cathodic inhibitor. The inhibition efficiency of naturally oil remains slightly constant with the rise of temperature. Chemical analysis of R.~officinalis essential oil was carried out using capillary GC and GC/MS. The oil composition was characterized by high amount of oxygenated monoterpene (77 %) with 1,8-cineol (52.1 %) as main component. Discussion of adsorption was investigated on the basis of essential oil composition. Finally, the isotherm adsorption of essential oil on the steel has been also reported.     

Transparent conducting properties of Ni doped zinc oxide thin films prepared by a facile spray pyrolysis technique using perfume atomizer

Undoped and Ni doped zinc oxide (Ni–ZnO) thin films were prepared by a facile spray pyrolysis technique using perfume atomizer from aqueous solution of anhydrous zinc acetate (Zn(CH₃COOH)₂ and hexahydrated nickel chloride (NiCl₂·6H₂O) as sources of zinc and nickel, respectively. The films were deposited onto the amorphous glass substrates kept at (450 °C). The effect of the [Ni]/[Zn] ratio on the structural, morphological, optical and electrical properties of Ni doped ZnO thin film was studied. It was found from X-ray diffraction (XRD) analysis that both the undoped and Ni doped ZnO films were crystallized in the hexagonal structure with a preferred orientation of the crystallites along the [002] direction perpendicular to the substrate. The scanning electron microscopy (SEM) images showed a relatively dense surface structure composed of crystallites in the spherical form whose average size decreases when the [Ni]/[Zn] ratio increases. The optical study showed that all the films were highly transparent. The optical transmittance in the visible region varied between 75 and 85%, depending on the dopant concentrations. The variation of the band gap versus the [Ni]/[Zn] ratio showed that the energy gap decreases from 2.95 to 2.72 eV as the [Ni]/[Zn] ratio increases from 0 to 0.02 and then increases to reach 3.22 eV for [Ni]/[Zn] = 0.04. The films obtained with the [Ni]/[Zn] ratio = 0.02 showed minimum resistivity of 2 × 10⁻³ Ω cm at room temperature.     

Synthesis and characterization of the new cellulose derivative films based on the hydroxyethyl cellulose prepared from “Stipa Tenacissima” cellulose of Eastern Morocco. I. Solubility study

Hydroxyethyl cellulose Acetate (HECA) was prepared starting from hydroxyethyl cellulose (HEC), acetic anhydride and perchloric acid which was used as catalyst. The synthesized product was characterized by FTIR, ¹³C NMR, and ¹H NMR. Substitution degree (DS) of HECA was determined using FTIR spectra taking a classical titration method as reference. The ¹H NMR spectroscopy was also used to confirm the results obtained by FTIR. The DS is substantially affected by the temperature, the time of reaction and especially the equivalent number (eq. nb.) of the acetic anhydride added. We have studied and discussed in the context of usage in modification reactions, the solubility of the HECA samples by varying their DS. This investigation was based on the determination of the Flory‐Huggins interaction parameters (χ_SP) using the partial Hansen solubility parameters (HSP). HSP of HEC and the HECA samples were calculated from the Van‐Krevlen‐Hoftyze (VKH) method and the T. Lindvig approximation. We have focused our work on predicting and controlling family solvents of HECA with various DS, to facilitate and to optimize the homogenous modification reaction conditions. From results on a range of HECA samples, it is conclude that their prediction solubility taking the value of DS into account is possible, and then the surface modification can relatively be easily realized. The thermal analysis study shows some differences in T_g and thermal degradation between HEC and HECA, moreover these thermal temperatures are influenced by DS values. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis and characterization of the new cellulose derivative films based on the hydroxyethyl cellulose prepared from esparto “stipa tenacissima” cellulose of Eastern Morocco. II. Esterification with acyl chlorides in a homogeneous medium

Esparto “Stipa tenacissima” cellulose esters derivatives: HECA‐COO? C₄H₈? COOC₂H₅, HECA‐COO? C₈H₁₆? COOC₂H₅, and HECA‐COO? C₆H₄? COOC₂H₅ were successfully prepared in Tetrahydrofuran (THF)/triethylamine system with a degree of substitution (DS), respectively, DS_AD‐Et=0.32, DS_SB‐Et=0.22, and DS_TRP‐Et=0.50 using hydroxyethyl cellulose acetate (HECA; DS_AC=0.50) as intermediate product, and we avoided the drawbacks of cellulose solubility. The structural modifications were investigated using Fourier transform infrared spectroscopy (FTIR), Proton nuclear magnetic resonance (¹H‐NMR), Carbon‐13 nuclear magnetic resonance (¹³C‐NMR), and Distortionless Enhancement by Polarization Transfer 135° (DEPT‐135). The results from these analyses revealed the presence of the characteristic groups indicating that the grafting reaction was successful. The crystallinity and the structure order changes during the esterification reactions were recorded by X‐ray diffraction (XRD), it is found that the crystallinity degree decrease from 63.1% for Esparto “Stipa tenacissima” cellulose to 27.74% for HECA. The thermal stability of the esterified and unmodified cellulose samples was studied by thermogravimetric analysis (TGA)‐differential thermal analysis (DTA); the modified HECA exhibits a decrease in thermal stability relatively to the unmodified HECA, and this may be related to the groups grafted. The resulted cellulose esters HECA‐P_x (x = 1, 2, or 3) were soluble in THF and present an amorphous structure justified by XRD spectra. It was noted by TGA‐DTA analysis that the cellulose esters with low melting range were proved as thermoplastic polymers. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

The effect of poly(vinyl caprolactone-co-vinyl pyridine) and poly(vinyl imidazol-co-vinyl pyridine) on the corrosion of steel in H<Subscript>3</Subscript>PO<Subscript>4</Subscript> media

The inhibiting effect of two organic copolymers namely poly(vinyl caprolactone-co-vinyl pyridine) (PVCVP) and poly(vinyl imidazol-co-vinyl pyridine) (PVIVP) on the corrosion of steel in phosphoric acid was investigated at various temperatures. The study was carried out by potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and weight loss measurements. Inhibition efficiency (E %) increased with polymer concentration to attain 85% at 10⁻⁴ M for PVIVP. Adsorption of polymers on the steel surface in 2 M H₃PO₄ followed the Langmuir isotherm model. EIS measurements show that the dissolution of steel occurs under activation control. Polarisation curves indicate that the tested polymers functioned as cathodic inhibitors. E % values obtained from various methods used are in good agreement with each other. The temperature effect on the corrosion behaviour of steel in 2 M H₃PO₄ in the presence and absence of the inhibitor was studied in the temperature range 298–338 K. The adsorption free energy (ΔG ^o _ads) and the activation parameters (E _a, , ΔS ^o _a) for the steel dissolution reaction in the presence of polymer were determined.