scholarly journals The Influence of Initiator Concentration on Selected Properties on Poly-N-Vinylcaprolactam Nanoparticles

Nanomaterials ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 1577
Author(s):  
Agnieszka Gola ◽  
Aleksandra Niżniowska ◽  
Witold Musiał

The thermosensitive polymers of N-vinylcaprolactam P1, P2, P3, P4, and P5 were synthesized via the surfactant free precipitation polymerization (SFPP) at 70 °C in the presence of cationic initiator 2,2’-azobis[2-methylpropionamidine] dihydrochloride (AMPA). The influence of various concentrations of initiator AMPA on particle size, aggregation and lower critical temperature solution (LCST) was investigated by dynamic light scattering (DLS) measurement. The conductivity was measured in the course of the synthesis and during temperature decrease of the reaction mixtures. The polymers were characterized by Attenuated Total Reflectance-Fourier Transform Infrared spectroscopy (ATR-FTIR), 1H NMR, and thermogravimetric analysis. Thermal parameters of the degradations process were investigated using thermogravimetric analysis (TGA/DTA) under non-isothermal conditions in N2 atmosphere. The samples were characterized by powder X-ray diffraction analysis (PXRD).The hydrodynamic diameter (HD), polydispersity index (PDI) and zeta potential (ZP) were measured in aqueous dispersions of the synthesized polymers in temperature 18–45 °C. HD and PDI values at 18 °C were 137.23 ± 67.65 nm (PDI = 0.53 ± 0.18), 83.40 ± 74.46 nm (PDI = 0.35 ± 0.08), 22.11 ± 0.29 nm (PDI = 0.45 ± 0.05), 29.27 ± 0.50 nm (PDI = 0.41 ± 0.04), 39.18 ± 0.57 nm (PDI = 0.38 ± 0.01) for P1, P2, P3, P4, and P5, respectively. The aqueous solutions of the obtained polymers at 18–45 °C had a positive charge. ZP’s for P1, P2, P3, P4, and P5 polymers at 18 °C were 11.64 ± 4.27 mV, 12.71 ± 3.56 mV, 3.24 ± 0.10 mV, 0.77 ± 0.28 mV, 1.78 ± 0.56 mV respectively. The LCST range was between 32 and 38 °C. We conclude that the concentration of initiator affects the size of obtained polymeric spheres and theirs LCST.

2014 ◽  
Vol 18 (1) ◽  
pp. 31-35
Author(s):  
Pey-Shin Ke ◽  
Wei-Jang Wu ◽  
Kuo-Shien Huang

We modified a basic dye, which carries a positive charge, by inducing an exchange with clay, and then analysed the results by using Fourier transform infrared (FT-IR) and ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The intercalation of basic dye into clay modifies the thermal properties of the dye, and the dyes become more stable as more clay is added. The colour of the modified dyes does not change with the addition of more clay, although its absorption decreases, thereby conferring improved sunlight colour fastness on the modified dyes.


Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 931
Author(s):  
Ioana-Codruţa Mirică ◽  
Gabriel Furtos ◽  
Ondine Lucaciu ◽  
Petru Pascuta ◽  
Mihaela Vlassa ◽  
...  

The aim of this research was to develop new electrospun membranes (EMs) based on polycaprolactone (PCL) with or without metronidazole (MET)/nano-hydroxyapatite (nHAP) content. New nHAP with a mean diameter of 34 nm in length was synthesized. X-ray diffraction (XRD) and attenuated total reflectance Fourier transform infrared spectroscopy (FTIR-ATR) were used for structural characterization of precursors and EMs. The highest mechanical properties (the force at maximum load, Young’s modulus and tensile strength) were found for the PCL membranes, and these properties decreased for the other samples in the following order: 95% PCL + 5% nHAP > 80% PCL + 20% MET > 75% PCL + 5% nHAP + 20% MET. The stiffness increased with the addition of 5 wt.% nHAP. The SEM images of EMs showed randomly oriented bead-free fibers that generated a porous structure with interconnected macropores. The fiber diameter showed values between 2 and 16 µm. The fiber diameter increased with the addition of nHAP filler and decreased when MET was added. New EMs with nHAP and MET could be promising materials for guided bone regeneration or tissue engineering.


Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4723
Author(s):  
Sara Dalle Vacche ◽  
Vijayaletchumy Karunakaran ◽  
Alessia Patrucco ◽  
Marina Zoccola ◽  
Loreleï Douard ◽  
...  

Nanocellulose was extracted from short bast fibers, from hemp (Cannabis sativa L.) plants harvested at seed maturity, non-retted, and mechanically decorticated in a defibering apparatus, giving non-aligned fibers. A chemical pretreatment with NaOH and HCl allowed the removal of most of the non-cellulosic components of the fibers. No bleaching was performed. The chemically pretreated fibers were then refined in a beater and treated with a cellulase enzyme, followed by mechanical defibrillation in an ultrafine friction grinder. The fibers were characterized by microscopy, infrared spectroscopy, thermogravimetric analysis and X-ray diffraction after each step of the process to understand the evolution of their morphology and composition. The obtained nanocellulose suspension was composed of short nanofibrils with widths of 5–12 nm, stacks of nanofibrils with widths of 20–200 nm, and some larger fibers. The crystallinity index was found to increase from 74% for the raw fibers to 80% for the nanocellulose. The nanocellulose retained a yellowish color, indicating the presence of some residual lignin. The properties of the nanopaper prepared with the hemp nanocellulose were similar to those of nanopapers prepared with wood pulp-derived rod-like nanofibrils.


2020 ◽  
Vol 75 (4) ◽  
pp. 365-369
Author(s):  
Long Tang ◽  
Yu Pei Fu ◽  
Na Cui ◽  
Ji Jiang Wang ◽  
Xiang Yang Hou ◽  
...  

AbstractA new metal-organic framework, [Pb(hmpcaH)2]n (1), has been hydrothermally synthesized from Pb(OAc)2 · 3H2O and 2-hydroxy-6-methylpyridine-4-carboxylic acid (hmpcaH2; 2), and characterized by IR spectroscopy, elemental and thermogravimetric analysis, and single-crystal X-ray diffraction. In complex 1, each hmpcaH− ligand represents a three-connected node to combine with the hexacoordinated Pb(II) ions, generating a 3D binodal (3,6)-connected ant network. The crystal structure of 2 was determined. The solid-state fluorescence properties of 1 and 2 were investigated.


Materials ◽  
2019 ◽  
Vol 12 (20) ◽  
pp. 3371 ◽  
Author(s):  
Svensson ◽  
Grins ◽  
Eklöf ◽  
Eriksson ◽  
Wardecki ◽  
...  

The CO2 adsorption on various Prussian blue analogue hexacyanoferrates was evaluated by thermogravimetric analysis. Compositions of prepared phases were verified by energy-dispersive X-ray spectroscopy, infra-red spectroscopy and powder X-ray diffraction. The influence of different alkali cations in the cubic Fm3m structures was investigated for nominal compositions A2/3Cu[Fe(CN)6]2/3 with A = vacant, Li, Na, K, Rb, Cs. The Rb and Cs compounds show the highest CO2 adsorption per unit cell, 3.3 molecules of CO2 at 20 C and 1 bar, while in terms of mmol/g the Na compound exhibits the highest adsorption capability, 3.8 mmol/g at 20 C and 1 bar. The fastest adsorption/desorption is exhibited by the A-cation free compound and the Li compound. The influence of the amount of Fe(CN)6 vacancies were assessed by determining the CO2 adsorption capabilities of Cu[Fe(CN)6]1/2 (Fm3m symmetry, nominally 50% vacancies), KCu[Fe(CN)6]3/4 (Fm3m symmetry, nominally 25% vacancies), and CsCu[Fe(CN)6] (I-4m2 symmetry, nominally 0% vacancies). Higher adsorption was, as expected, shown on compounds with higher vacancy concentrations.


2021 ◽  
Vol 875 ◽  
pp. 116-120
Author(s):  
Muhammad Alamgir ◽  
Faizan Ali Ghauri ◽  
Waheed Qamar Khan ◽  
Sajawal Rasheed ◽  
Muhammad Sarfraz Nawaz ◽  
...  

In this study, the effect of SBR concentration (10 Phr, 20 Phr & 30 Phr ) on the thermal behavior of EPDM/SBR blends was studied. Thermogravimetric analysis (TGA) was used to check weight loss of samples as function of temperature by heating upto 600°C. X-ray diffraction (XRD) was performed to determine quality and % crystallinity of the elastomer blends. It was seen that % crystallinity improved with an increase in the content of SBR in EPDM/SBR blends. TGA revealed that the thermal stability of EPDM/SBR blends has improved by 17% than neat EPDM. Carbon nano-coatings produced by sputtering have no beneficial influence on thermal behaviour of elastomers.


2012 ◽  
Vol 727-728 ◽  
pp. 1467-1472
Author(s):  
Carla Dantas da Silva ◽  
Rosa do Carmo de Oliveira Lima ◽  
Julliana Marques Rocha Costa ◽  
Gelmires Araújo Neves ◽  
Heber Carlos Ferreira

This work aims at the development of organoclay from two varieties of bentonite for use in organic media using ionic surfactants, studying the influence of process variables in the organophilization process. We used the following materials: natural bentonite clay from Cubati-PB District, and the ionic quaternary ammonium salt: Praepagen WB® with 45% active matter. The clays were benefited and then turned into sodium form and subsequently into organoclays. The bentonites were characterized by laser diffraction (GA) X-ray fluorescence chemical composition (EDX), thermogravimetric analysis (TGA), thermogravimetry (DTA) and X-ray diffraction (XRD). The organoclays were characterized by (XRD) thermogravimetric analysis (TGA) and thermogravimetry (DTA). The results showed that the clay has potential for application in the organophilization process and that there is influence of process variables.


2019 ◽  
Vol 19 (1) ◽  
pp. 83-99 ◽  
Author(s):  
B. Yilmaz ◽  
E. T. Irmak ◽  
Y. Turhan ◽  
S. Doğan ◽  
M. Doğan ◽  
...  

AbstractThe aims of the present study were to synthesize the intercalated kaolinite samples with dimethylsulfoxide (DMSO), glutamic acid (GA), succinimide (SIM), cetylpyridiniumchloride (CPC), and hexadecyltrimethylammoniumchloride (HDTMA+); to characterize by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR), and to determine the hemocompatibility and the cytotoxic effects of the intercalated kaolinite nanoclays on human lymphocytes. It was found that the intercalation with DMSO did not cause any decrease in cell viability until its maximum concentration (500 µg/mL), however, the intercalation with SIM, CPC, and (HDTMA+) causd important decreases in lymphocyte viabilities. It was determined that no significant decrease was observed in protein content of the lymphocyte cells exposed to the kaolinite nanoclays except the ones intercalated with SIM. Furthermore, the pristine kaolinite nanoclays which were intercalated with DMSO, GA, and SIM exhibited high hemocompatibility and the nanoclays intercalated with CPC and (HDTMA+) were highly hemocompatibile for the amounts below 125 and 500 µg/mL, respectively. All the results of this work can serve for the human risk assesment of intercalated nanoclays.


2008 ◽  
Vol 569 ◽  
pp. 45-48
Author(s):  
Hai Yun Jin ◽  
Guan Jun Qiao ◽  
Zong Ren Peng ◽  
Ji Qiang Gao

SiC particles coated with nano-BN were synthesized and the machinable SiC/BN ceramic nano-composites were fabricated by Plasma Active Sintering (PAS) in N2 atmosphere. The existing and distribution of h-BN phase were revealed by X-ray diffraction (XRD), and SEM. For the existing of weak interface between h-BN and SiC grains, the machinability of both SiC/BN micro-composites and nano-composites were improved obviously. Because the nano-sized h-BN crystals were homogeneously dispersed around the SiC grains of the matrix, the fracture strength of the nano-composites was better than the SiC/h-BN micro-composite.


1999 ◽  
Vol 14 (3) ◽  
pp. 219-221 ◽  
Author(s):  
V. Venegas ◽  
A. Gómez ◽  
E. Reguera

The crystal structure of disilver(1+) pentacyanonitrosylferrate(2−) was studied by X-ray powder diffraction. IR and Mössbauer spectroscopies, thermogravimetric analysis and density measurements were also carried out. This compound is monoclinic, and its lattice parameters are: a=10.986(3) Å, b=6.4080(10) Å, c=7.4545(19) Å, α=δ=90°, β=102.54°(2).


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