Preparation and characterization of 1,2,4,5-benzenetetra carboxylic-chitosan

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Nurhidayatullaili Muhd Julkapli ◽  
Zulkifli Ahmad ◽  
Hazizan Md Akil

AbstractChemically cross-linked chitosan (MC) containing 1,2,4,5- benzenetetracarboxylic acid (BCA) as the cross-linking agent was prepared to improve the metal ions absorption capacity of native chitosan (NC) and limit its biodegradability. The Fourier transform infra-red (FTIR) and proton neutron magnetic resonance (1H NMR) results showed that BCA was successfully linked onto N-position of NC. The crystalline nature of NC was reduced significantly after cross-linking as examined by X-ray diffraction (XRD) analysis. Therefore, the glass transition temperature (Tg) of MC was higher than NC as reported by differential scanning calorimetry (DSC). Moreover, thermogravimetric (TGA) analysis showed that, MC had better thermal stability than NC. Morphology changes on the surface of NC and MC were characterized by field emission scanning electron microscopy (FESEM) and showed that MC had more porous surface than NC. In pH medium of 3 to 6, MC had excellent Cu (II) ions absorption capacity with a maximum 16 % higher than NC.

2021 ◽  
Vol 2129 (1) ◽  
pp. 012092
Author(s):  
Suffi Irni Alias ◽  
Banjuraizah Johar ◽  
Syed Nuzul Fadzli Adam ◽  
Mustaffa Ali Azhar Taib ◽  
Fatin Fatini Othman ◽  
...  

Abstract The porcelain formulation containing percentages of treated FGD sludge waste from 5% up to 15% in replacement of feldspar were prepared. The porcelain mixture formulation were mixed by high energy planatery mill at speed 300 rpm for 1 hours. The powder were compacted by using hydraulic press and sintered at temperature 1200 °C for 3 hours. The sintered samples were characterized using X-ray fluorescene (XRF), X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) and Thermogravimetry/Differential scanning calorimetry (TGA/DCS). The primary effect concerning the addition of treated FGD sludge was the change of intensity composition (gypsum and anhydrate) in porcelain formulation. The XRD analysis has shown that the main component in sludge waste were gypsum and anhydrate.


2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Hao Ding ◽  
Yuebo Wang ◽  
Yu Liang ◽  
Faxiang Qin

Intercalated sericite was prepared by intercalation of cetyl trimethylammonium bromide (CTAB) into activated sericite through ion exchange with the following two steps: the activation of sericite by thermal modification, acid activation and sodium modification; the ion exchange intercalation of CTA+into activated sericite. Effects of reaction time, reaction temperature, CTAB quantity, kinds of medium, and aqueous pH on the intercalation of activated sericite were examined by X-ray diffraction (XRD) analysis, Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The results indicated that the CTA+entered sericite interlayers and anchored in the aluminosilicate interlayers through strong electrostatic attraction. The arrangement of CTA+in sericite interlayers was that alkyl chain of CTA+mainly tilted at an angle about 60° (paraffin-type bilayer) and 38° (paraffin-type monolayer) with aluminosilicate layers. The largest interlayer space was enlarged from 0.9 nm to 5.2 nm. The intercalated sericite could be used as an excellent layer silicate to prepare clay-polymer nanocomposites.


e-Polymers ◽  
2008 ◽  
Vol 8 (1) ◽  
Author(s):  
Ahmad Banihashemi ◽  
Mohammad Reza Vakili

AbstractA pyridine-based diacid containing ether linkage was synthesized via reaction of 2,6-dichloropyridine with 3-hydroxybenzoic acid in presence of potassium hydroxide in dimethyl sulfoxide (DMSO). The corresponding diacid chloride was synthesized by reaction of the diacid with oxalyl chloride. New poly (amide-ether)s were prepared by solution polycondensation reaction of the prepared diacid chloride with different commercial aromatic diamines. The synthesized polymers were characterized by elemental analysis, IR, and 1H NMR spectra, wide-angle X-ray diffraction, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC); inherent viscosity and solubility were studied. These polymers showed high thermal stability and good solubility.


Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.


Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 721 ◽  
Author(s):  
Jorge A. Ramírez-Gómez ◽  
Javier Illescas ◽  
María del Carmen Díaz-Nava ◽  
Claudia Muro-Urista ◽  
Sonia Martínez-Gallegos ◽  
...  

Atrazine (ATZ) is an herbicide which is applied to the soil, and its mechanism of action involves the inhibition of photosynthesis. One of its main functions is to control the appearance of weeds in crops, primarily in corn, sorghum, sugar cane, and wheat; however, it is very toxic for numerous species, including humans. Therefore, this work deals with the adsorption of ATZ from aqueous solutions using nanocomposite materials, synthesized with two different types of organo-modified clays. Those were obtained by the free radical polymerization of 4-vinylpyridine (4VP) and acrylamide (AAm) in different stoichiometric ratios, using tetrabutylphosphonium persulfate (TBPPS) as a radical initiator and N,N′-methylenebisacrylamide (BIS) as cross-linking agent. The structural, morphological, and textural characteristics of clays, copolymers, and nanocomposites were determined through different analytical and instrumental techniques, i.e., X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Adsorption kinetics experiments of ATZ were determined with the modified and synthesized materials, and the effect of the ratio between 4VP and AAm moieties on the removal capacities of the obtained nanocomposites was evaluated. Finally, from these sets of experiments, it was demonstrated that the synthesized nanocomposites with higher molar fractions of 4VP obtained the highest removal percentages of ATZ.


2020 ◽  
Vol 849 ◽  
pp. 113-118
Author(s):  
Yayat Iman Supriyatna ◽  
Slamet Sumardi ◽  
Widi Astuti ◽  
Athessia N. Nainggolan ◽  
Ajeng W. Ismail ◽  
...  

The purpose of this study is to characterize Lampung iron sand and to conduct preliminary experiments on the TiO2 synthesis which can be used for the manufacturing of functional food packaging. The iron sand from South Lampung Regency, Lampung Province that will be utilized as raw material. The experiment was initiated by sieving the iron sand on 80, 100, 150, 200 and 325 mesh sieves. Analysis using X-Ray Fluorescence (XRF) to determine the element content and X-Ray Diffraction (XRD) to observe the mineralization of the iron sand was conducted. The experiment was carried out through the stages of leaching, precipitation, and calcination. Roasting was applied firstly by putting the iron sand into the muffle furnace for 5 hours at a temperature of 700°C. Followed by leaching using HCl for 48 hours and heated at 105°C with a stirring speed of 300 rpm. The leaching solution was filtered with filtrate and solid residue as products. The solid residue was then leached using 10% H2O2 solution. The leached filtrate was heated at 105°C for 40 minutes resulting TiO2 precipitates (powder). Further, the powder was calcined and characterized. Characterization of raw material using XRF shows the major elements of Fe, Ti, Mg, Si, Al and Ca. The highest Ti content is found in mesh 200 with 9.6%, while iron content is about 80.7%. While from the XRD analysis, it shows five mineral types namely magnetite (Fe3O4), Rhodonite (Mn, Fe, Mg, Ca) SiO3, Quart (SiO2), Ilmenite (FeOTiO2) and Rutile (TiO2). The preliminary experiment showed that the Ti content in the synthesized TiO2 powder is 21.2%. The purity of TiO2 is low due to the presence of Fe metal which is dissolved during leaching, so that prior to precipitation purification is needed to remove impurities such as iron and other metals.


e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.


2018 ◽  
Vol 22 (09n10) ◽  
pp. 814-820
Author(s):  
Yingying Jia ◽  
Ling Xu ◽  
Bangshao Yin ◽  
Mingbo Zhou ◽  
Jianxin Song

Beginning with 5,10,15-triarylporphyrin-nickel complex, five meso-to-meso directly linked porphyrin-diazaporphyrin triads were successfully prepared for the first time through a series of reactions including formylation via Vilsmeier–Haack reaction, condensation with pyrrole, bromination with [Formula: see text]-Bromosuccinimide (NBS), oxidation with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), metal-templated cyclization of dibromodipyrrin-metal complexes with NaN[Formula: see text] and demetalization. All these triads were comprehensively characterized by [Formula: see text]H NMR, high-resolution mass spectrometry and UV-vis absorption. In addition, the structure of compound 6Ni was unambiguously determined by X-ray diffraction analysis, which showed that the two dihedral angles are both 86.65 (4)[Formula: see text] between each mean plane of porphyrin and that of central diazaporphyrin The UV-vis absorption spectra disclosed that the longest wavelengths of Soret bands and Q bands for these triads were observed at 429 and 642 nm, respectively. In contrast to diazaporphyrin-porphyrin dyads, diazaporphyrin dimers and diazaporphyrin monomers reported previously the molar extinction coefficients, particularly for triad 8Ni are much higher.


Materials ◽  
2020 ◽  
Vol 13 (13) ◽  
pp. 3035
Author(s):  
Dovydas Karoblis ◽  
Diana Griesiute ◽  
Kestutis Mazeika ◽  
Dalis Baltrunas ◽  
Dmitry V. Karpinsky ◽  
...  

In this study, a highly crystalline bismuth ferrite (BFO) powder was synthesized using a novel, very simple, and cost-effective synthetic approach. It was demonstrated that the optimal annealing temperature for the preparation of highly-pure BFO is 650 °C. At lower or higher temperatures, the formation of neighboring crystal phases was observed. The thermal behavior of BFO precursor gel was investigated by thermogravimetric and differential scanning calorimetry (TG-DSC) measurements. X-ray diffraction (XRD) analysis and Mössbauer spectroscopy were employed for the investigation of structural properties. Scanning electron microscopy (SEM) was used to evaluate morphological features of the synthesized materials. The obtained powders were also characterized by magnetization measurements, which showed antiferromagnetic behavior of BFO powders.


Author(s):  
S. Louki ◽  
N. Touach ◽  
A. Benzaouak ◽  
V. M. Ortiz-Martínez ◽  
M. J. Salar-García ◽  
...  

This work investigates the photocatalytic activity of new ferroelectric material with formula (Li0.95Cu0.15)Ta0.76Nb0.19O3 (LT76) in a single chamber microbial fuel cell (MFC) and compares its performance with the similar photocatalyst (Li0.95Cu0.15)Ta0.57Nb0.38O3 (LT57). The photocatalysts LT76 and LT57 were synthesized by ceramic route under the same conditions, with the same starting materials. The ratio Ta/Nb was fixed at 4.0 and 1.5 for LT76 and LT57, respectively. These phases were characterized by different techniques including X-ray diffraction (XRD), transmission electronic microscopy (TEM), particle size distribution (PSD), differential scanning calorimetry (DSC), and ultraviolet (UV)–visible (Vis). The new photocatalyst LT76 presents specific surface area of 0.791 m2/g and Curie temperature of 1197 °C. The photocatalytic efficiency of this material is assessed in terms of wastewater treatment and electricity generation by power density and removal rate of chemical oxygen demand (COD) in the presence of a light source. The values of maximum power density and COD removal were 19.77 mW/m3 and 93%, respectively, for LT76.


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