scholarly journals Synthesis of Epoxy Methacrylate Resin and Coatings Preparation by Cationic and Radical Photocrosslinking

Molecules ◽  
2021 ◽  
Vol 26 (24) ◽  
pp. 7663
Author(s):  
Paulina Bednarczyk ◽  
Izabela Irska ◽  
Konrad Gziut ◽  
Paula Ossowicz-Rupniewska
Keyword(s):  
Radical Polymerization ◽  
Acid Value ◽  
Synthesis Process ◽  
Initial Reaction ◽  
High Concentration ◽  
Scanning Calorimetry ◽  
Synthesis Time ◽  
Low Viscosity ◽  
Industrial Grade ◽  
Ft Ir

This work involves the synthesis of hybrid oligomers based on the epoxy methacrylate resin. The EA resin was obtained by the modification of industrial-grade bisphenol A-based epoxy resin and methacrylic acid has been synthesized in order to develop multifunctional resins comprising both epoxide group and reactive, terminal unsaturation. Owing to the presence of both epoxy and double carbon–carbon pendant groups, the reaction product exhibits photocrosslinking via two distinct mechanisms: (i) cationic ring-opening polymerization and (ii) free radical polymerization. Monitoring of EA synthesis reactions over time using PAVs, MAAC and NV parameters, and the FT-IR method reveals that esterification reactions proceed faster at the start, exhibiting over 40% of conversion within the initial 60 min, which can be associated with a relatively high concentration of reactive sites and low viscosity of the reaction mixture at the initial reaction stage. With the further increase in the reaction time, the reaction rate tends to decrease.. The control of the EA synthesis process can guide how to adjust reactions to obtain EAs with desired characteristics. Based on obtained values, one can state that the optimum synthesis time of about 4–5 h should be adopted to prepare EAs having both epoxy groups and unsaturated double bonds. The structure of the obtained EA was confirmed by FT-IR and NMR methods, as well as the determination of partial acid value and epoxy equivalent. Samples at various stages of synthesis were cured with UV radiation in order to study the kinetics of the process according to cationic and radical polymerization determined via photo-differential scanning calorimetry (photo-DSC) and real-time infrared spectroscopy (RT-IR) and then the properties of the cured coatings were tested. It turned out that the cationic polymerization was slower with a lower conversion of the photoreactive groups, as compared to the radical polymerization. All the obtained EA coatings were characterized by good properties of cured coatings and can be successfully used in the coating-forming sector.

scholarly journals Photocurable Epoxy Acrylate Coatings Preparation by Dual Cationic and Radical Photocrosslinking

Materials ◽  
2021 ◽  
Vol 14 (15) ◽  
pp. 4150
Author(s):  
Paulina Bednarczyk ◽  
Karolina Mozelewska ◽  
Małgorzata Nowak ◽  
Zbigniew Czech
Keyword(s):  
Free Radical ◽  
Radical Polymerization ◽  
Free Radical Polymerization ◽  
Hybrid Coatings ◽  
Epoxy Acrylate ◽  
Structural Factors ◽  
Scanning Calorimetry ◽  
Yellowness Index ◽  
Hybrid Resin ◽  
Industrial Grade

In this work, epoxy acrylate resin (EA) based on the industrial-grade bisphenol A-based epoxy resin (Ep6) and acrylic acid (AA) has been synthesized in order to develop hybrid resin comprising both epoxide group and reactive, terminal unsaturation. Obtained epoxy acrylate prepolymer was employed to formulate photocurable coating compositions containing, besides the EA binder, also cationic or radical photoinitiators. Hence, when cationic photoinitiators were applied, polyether-type polymer chains with pending acrylate groups were formed. In the case of free radical polymerization, epoxy acrylates certainly formed a polyacrylate backbone with pending epoxy groups. Owing to the presence of both epoxy and double carbon–carbon pendant groups, the reaction product exhibits photocrosslinking via two distinct mechanisms: (i) cationic ring-opening polymerization and (ii) free radical polymerization. Therefore, photopolymerization behavior of synthetized hybrid resin with various photoinitiators was determined via photo-differential scanning calorimetry (photo-DSC) and real-time infrared spectroscopy (RT-IR) methods, and properties of cured coatings were investigated. The performance of the following type of photoinitiators was tested in the cationic photopolymerization: diaryliodonium cations or triarylsulfonium cations, and the following type of photoinitiators were used to induce free radical photopolymerization: α-hydroxyketones, acylphosphine oxides, and their mixtures. Lastly, the basic physicomechanical properties of cured coatings, such as tack-free time, hardness, adhesion, gloss, and yellowness index, were evaluated. Some structural factors and parameters of cationic and radical photoinitiators and photopolymerization mechanisms affecting the epoxy acrylate hybrid coatings performance are discussed.

scholarly journals Some variables affecting the characteristics of Eudragit E-sodium alginate polyelectrolyte complex as a tablet matrix for diltiazem hydrochloride

2014 ◽  
Vol 64 (1) ◽  
pp. 89-104 ◽  
Author(s):  
Rehab Mohammad Yusif ◽  
Irhan Ibrahim Abu Hashim ◽  
Marwa Salah El-Dahan
Keyword(s):  
Sodium Alginate ◽  
Diltiazem Hydrochloride ◽  
Scanning Calorimetry ◽  
Polyelectrolyte Complexes ◽  
Low Viscosity ◽  
Eudragit E ◽  
Swelling Characteristics ◽  
Ft Ir ◽  
Physical Mixtures

Abstract Eudragit E (EE)-sodium alginate (SA) polyelectrolyte complexes (PECs) were prepared at pH 4 and 5.8 using sodium alginate of high (SAH) and low viscosity (SAL). The optimum EE-SA complexation mass ratio was determined using viscosity measurements. Interactions between EE and SA in PECs were characterized by Fourier transform infra-red spectroscopy (FT-IR) and differential scanning calorimetry (DSC). Diltiazem hydrochloride (DTZ HCl) tablets were prepared using the prepared EE-SA PECs and their physical mixtures at different ratios as matrices. Tablets were evaluated for swelling characteristics and in vitro drug release. Tablets containing EE-SAH physical mixtures of ratios (1.5:1 and 1:3) as matrices were effective in achieving sustained release of DTZ HCl, where the percent drug released was significantly (p < 0.05) decreased compared to that from tablets either containing the same ratios of EE-SAL physical mixtures or the preformed EE- -SAH and EE-SAL PECs.

scholarly journals Performance of urea-formaldehyde adhesive with oxidized cassava starch

BioResources ◽  
2017 ◽  
Vol 12 (4) ◽  
pp. 7590-7600
Author(s):  
Hui Wang ◽  
Jiankun Liang ◽  
Jun Zhang ◽  
Xiaojian Zhou ◽  
Guanben Du
Keyword(s):  
Urea Formaldehyde ◽  
Negative Relationship ◽  
Cassava Starch ◽  
Solid Content ◽  
Synthesis Process ◽  
Scanning Calorimetry ◽  
Curing Characteristics ◽  
13C Nmr Analysis ◽  
Ft Ir ◽  
Basic Characteristics

Urea-formaldehyde (UF) resins based on different formaldehyde/urea (F/U) mole ratio were synthesized with oxidized cassava starch added at the final stage of the resin synthesis process. The basic characteristics of resins including solid content, viscosity, and curing time were studied, and the dry and wet bond strengths were evaluated by producing a three layer plywood. Additionally, the curing characteristics of different resins were investigated via differential scanning calorimetry (DSC). Structural distributions between UF and oxidized cassava starch were examined via FT-IR and 13C NMR analysis. The results indicated that the addition of oxidized starch not only improved resin bond strength but also notably reduced the curing start temperature of modified resins. Furthermore, a negative relationship between F/U mole ratio and the extent of reduction was identified. The structural distribution of UF resins changed dramatically because of oxidation cassava starch addition, but the changes varied due to different F/U mole ratios.

scholarly journals The research determines appropriate parameters in the synthesis process of syringic acid grafted chitooligosaccharides

2019 ◽  
Vol 22 (3) ◽  
pp. 317-323
Author(s):  
Hoai Van Bui ◽  
Nghiep Dai Ngo
Keyword(s):  
Hydrogen Peroxide ◽  
Ascorbic Acid ◽  
Pathogenic Bacteria ◽  
Syringic Acid ◽  
Synthesis Process ◽  
Mass Ratio ◽  
Synthesis Time ◽  
Redox Pair ◽  
Ft Ir ◽  
Grafting Degree

Introduction: The aim of this study is to determine appropriate parameters in the synthesis of syringic acid onto chitooligosaccharides (COSs) with an ascorbic acid/hydrogen peroxide redox pair in order to obtain the derivative with the highest grafting degree. Methods: In this study, syringic acid grafted COSs, catalysed by an ascorbic acid/hydrogen peroxide redox pair were investigated. The synthesis conditions were investigated, including the mass ratio between syringic acid and COSs, pH, temperature and synthesis time. Characteristics of the derivative were evaluated by Thin Layer Chromatography (TLC), Ultraviolet-Visible (UV-vis) and Fourier Transform Infrared (FT-IR) spectroscopy. The activities of COSs and derivative were evaluated by antimicrobial ability. Results: The results showed, that the best conditions for the synthesis were the mass ratio between syringic acid and COSs at 0.5:1, pH 5, temperature 27oC, for 6 hours with grafting degree at 32%. The TLC assay showed, that free ascorbic acid and syringic acid are not present in the product. The UV-vis and FT-IR data confirmed, that syringic acid was successfully conjugated onto COSs. Furthermore, the antibacterial assay showed that syringic acid grafted onto COSs had minimum inhibitory concentration against foodborne pathogenic bacteria at 1%. Conclusion: The syringic acid onto chitooligosaccharides were successfully synthesized by free radical mediated grafting method with an ascorbic acid/hydrogen peroxide redox pair. The grafting degree of syringic acid onto COSs was greatly affected by many factors, including COSs, syringic acid, pH, as well as temperature and time of reaction. Moreover, the new derivative showed enhanced antibacterial capabilities, as compare to free COSs.  

scholarly journals Morphological, Mechanical and Physio-chemical Performance of ortho-Cresol Epoxy Novolac Based Vinyl Ester Resin

2015 ◽  
Vol 17 (3) ◽  
pp. 1-7
Author(s):  
Shipra Jaswal ◽  
Bharti Gaur
Keyword(s):  
Epoxy Resin ◽  
Vinyl Ester ◽  
Testing Machine ◽  
Acid Value ◽  
Vinyl Ester Resin ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Reactive Diluents ◽  
Ft Ir ◽  
Ortho Cresol

Abstract Vinyl ester resin (VEOCN) was prepared from o-cresol epoxy resin (EOCN) and methacrylic acid in the presence of triphenyl phosphine as catalyst and hydroquinone as inhibitor with acid value of ~ 7 mg of KOH per gram of solid. O-cresol based novolac resin (OCN), OCN based epoxy resin (EOCN) and VEOCN were characterized by Fourier transform infra red spectroscopy (FT-IR), 1H-NMR and 13C-NMR. The thermal and mechanical behavior of the samples prepared at 30°C from VEOCN using styrene and methyl-methacrylate respectively as reactive diluents, in the presence of benzoyl peroxide (2 phr) as initiator was studied using Differential Scanning Calorimetry (DSC), Thermogravimetric analysis (TGA) and Universal Testing Machine (UTM). Chemical resistance of above VER samples was also evaluated as a function of % weight loss and with the help of Scanning Electron Microscopy (SEM), upon immersing the VEOCN samples in different solutions for 90 days.

Thermal Behaviour of Candesartan Active substance and in pharmaceutical compounds

2017 ◽  
Vol 68 (8) ◽  
pp. 1895-1902
Author(s):  
Ioana Cristina Tita ◽  
Eleonora Marian ◽  
Bogdan Tita ◽  
Claudia Crina Toma ◽  
Laura Vicas
Keyword(s):  
Thermal Behaviour ◽  
Active Substance ◽  
Pharmaceutical Research ◽  
Pharmaceutical Product ◽  
Nitrogen Atmosphere ◽  
Pure Substance ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir

Thermal analysis is one of the most frequently used instrumental techniques in the pharmaceutical research, for the thermal characterization of different materials from solids to semi-solids, which are of pharmaceutical relevance. In this paper, simultaneous thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC) were used for characterization of the thermal behaviour of candesartan cilexetil � active substance (C-AS) under dynamic nitrogen atmosphere and nonisothermal conditions, in comparison with pharmaceutical product containing the corresponding active substance. It was observed that the commercial samples showed a different thermal profile than the standard sample, caused by the presence of excipients in the pharmaceutical product and to possible interaction of these with the active substance. The Fourier transformed infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRPD) were used as complementary techniques adequately implement and assist in interpretation of the thermal results. The main conclusion of this comparative study was that the TG/DTG and DSC curves, together with the FT-IR spectra, respectively X-ray difractograms constitute believe data for the discrimination between the pure substance and pharmaceutical forms.

The Development of Pemetrexed Diacid-Loaded Gelatin-Cloisite 30B (MMT) Nanocomposite for Improved Oral Efficacy Against Cancer: Characterization, In-Vitro and Ex-Vivo Assessment

2020 ◽  
Vol 17 (3) ◽  
pp. 246-256
Author(s):  
Kriti Soni ◽  
Ali Mujtaba ◽  
Md. Habban Akhter ◽  
Kanchan Kohli
Keyword(s):  
Drug Release ◽  
Oral Delivery ◽  
Ex Vivo ◽  
Confocal Laser ◽  
Release Mechanism ◽  
Scanning Calorimetry ◽  
Sem Images ◽  
Cloisite 30B ◽  
Ft Ir

Aim: The intention of this investigation was to develop Pemetrexed Diacid (PTX)-loaded gelatine-cloisite 30B (MMT) nanocomposite for the potential oral delivery of PTX and the in vitro, and ex vivo assessment. Background: Gelatin/Cloisite 30 B (MMT) nanocomposites were prepared by blending gelatin with MMT in aqueous solution. Methods: PTX was incorporated into the nanocomposite preparation. The nanocomposites were investigated by Fourier Transmission Infra Red Spectroscopy (FT-IR), Differential Scanning Calorimetry (DSC), Scanning Electron Microscope (SEM) X-Ray Diffraction (XRD) and Confocal Laser Microscopy (CLSM). FT-IR of nanocomposite showed the disappearance of all major peaks which corroborated the formation of nanocomposites. The nanocomposites were found to have a particle size of 121.9 ± 1.85 nm and zeta potential -12.1 ± 0.63 mV. DSC thermogram of drug loaded nanocomposites indicated peak at 117.165 oC and 205.816 oC, which clearly revealed that the drug has been incorporated into the nanocomposite because of cross-linking of cloisite 30 B and gelatin in the presence of glutaraldehyde. Results: SEM images of gelatin show a network like structure which disappears in the nanocomposite. The kinetics of the drug release was studied in order to ascertain the type of release mechanism. The drug release from nanocomposites was in a controlled manner, followed by first-order kinetics and the drug release mechanism was found to be of Fickian type. Conclusion: Ex vivo gut permeation studies revealed 4 times enhancement in the permeation of drug present in the nanocomposite as compared to plain drug solution and were further affirmed by CLSM. Thus, gelatin/(MMT) nanocomposite could be promising for the oral delivery of PTX in cancer therapy and future prospects for the industrial pharmacy.

Crystal Transition and Drug-excipient Compatibility of Clarithromycin in Sustained Release Tablets

2020 ◽  
Vol 16 (7) ◽  
pp. 950-959
Author(s):  
Yu Li ◽  
Xiangwen Kong ◽  
Fan Hu
Keyword(s):  
Sustained Release ◽  
Powder Diffraction ◽  
Magnesium Stearate ◽  
Influential Factor ◽  
High Concentration ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Sustained Release Tablets ◽  
Crystal Transition ◽  
Excipient Compatibility

Background: Clarithromycin is widely used for infections of helicobacter pylori. Clarithromycin belongs to polymorphic drug. Crystalline state changes of clarithromycin in sustained release tablets were found. Objective: The aim of this study was to find the influential factor of the crystal transition of clarithromycin in preparation process of sustained-release tablets and to investigate the possible interactions between the clarithromycin and pharmaceutical excipients. Methods and Results: The crystal transition of active pharmaceuticals ingredients from form II to form I in portion in clarithromycin sustained release tablets were confirmed by x-ray powder diffraction. The techniques including differential scanning calorimetry and infrared spectroscopy, x-ray powder diffraction were used for assessing the compatibility between clarithromycin and several excipients as magnesium stearate, lactose, sodium carboxymethyl cellulose, polyvinyl-pyrrolidone K-30 and microcrystalline cellulose. All of these methods showed compatibilities between clarithromycin and the selected excipients. Alcohol prescription simulation was also done, which showed incompatibility between clarithromycin and concentration alcohol. Conclusion: It was confirmed that the reason for the incompatibility of clarithromycin with high concentration of alcohol was crystal transition.

scholarly journals Optimization of the Production Process and Product Quality of Titanate Nanotube–Drug Composites

Nanomaterials ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 1406 ◽  
Author(s):  
Yasmin Ranjous ◽  
Géza Regdon ◽  
Klára Pintye-Hódi ◽  
Tamás Varga ◽  
Imre Szenti ◽  
...  
Keyword(s):  
Scanning Calorimetry ◽  
Good Solubility ◽  
Composite Formation ◽  
Alternative Materials ◽  
High Volatility ◽  
Ft Ir ◽  
Fast Disintegrating Tablets ◽  
As Solubility ◽  
Properties Of Composites

Recently, there has been an increasing interest in the application of nanotubular structures for drug delivery. There are several promising results with carbon nanotubes; however, in light of some toxicity issues, the search for alternative materials has come into focus. The objective of the present study was to investigate the influence of the applied solvent on the composite formation of titanate nanotubes (TNTs) with various drugs in order to improve their pharmacokinetics, such as solubility, stability, and bioavailability. Composites were formed by the dissolution of atenolol (ATN) and hydrochlorothiazide (HCT) in ethanol, methanol, 0.01 M hydrochloric acid or in ethanol, 1M sodium hydroxide, dimethylformamide (DMF), dimethyl sulfoxide (DMSO), respectively, and then they were mixed with a suspension of TNTs under sonication for 30 min and vacuum-dried for 24 h. The structural properties of composites were characterized by SEM, TEM, FT-IR, differential scanning calorimetry (DSC), thermogravimetric (TG) analysis, and optical contact angle (OCA) measurements. Drug release was determined from the fast disintegrating tablets using a dissolution tester coupled with a UV–Vis spectrometer. The results revealed that not only the good solubility of the drug in the applied solvent, but also the high volatility of the solvent, is necessary for an optimal composite-formation process.

scholarly journals Extraction of sugarcane bagasse arabinoxylan, integrated with enzymatic production of xylo-oligosaccharides and separation of cellulose

2021 ◽  
Vol 14 (1) ◽  
Author(s):  
Leila Khaleghipour ◽  
Javier A. Linares-Pastén ◽  
Hamid Rashedi ◽  
Seyed Omid Ranaei Siadat ◽  
Andrius Jasilionis ◽  
...  
Keyword(s):  
Sugarcane Bagasse ◽  
Sugar Content ◽  
Value Added ◽  
Apparent Molecular Weight ◽  
Bacillus Halodurans ◽  
Glycoside Hydrolase Family ◽  
High Concentration ◽  
Enzymatic Production ◽  
Successful Separation ◽  
Ft Ir

AbstractSugarcane processing roughly generates 54 million tonnes sugarcane bagasse (SCB)/year, making SCB an important material for upgrading to value-added molecules. In this study, an integrated scheme was developed for separating xylan, lignin and cellulose, followed by production of xylo-oligosaccharides (XOS) from SCB. Xylan extraction conditions were screened in: (1) single extractions in NaOH (0.25, 0.5, or 1 M), 121 °C (1 bar), 30 and 60 min; (2) 3 × repeated extraction cycles in NaOH (1 or 2 M), 121 °C (1 bar), 30 and 60 min or (3) pressurized liquid extractions (PLE), 100 bar, at low alkalinity (0–0.1 M NaOH) in the time and temperature range 10–30 min and 50–150 °C. Higher concentration of alkali (2 M NaOH) increased the xylan yield and resulted in higher apparent molecular weight of the xylan polymer (212 kDa using 1 and 2 M NaOH, vs 47 kDa using 0.5 M NaOH), but decreased the substituent sugar content. Repeated extraction at 2 M NaOH, 121 °C, 60 min solubilized both xylan (85.6% of the SCB xylan), and lignin (84.1% of the lignin), and left cellulose of high purity (95.8%) in the residuals. Solubilized xylan was separated from lignin by precipitation, and a polymer with β-1,4-linked xylose backbone substituted by arabinose and glucuronic acids was confirmed by FT-IR and monosaccharide analysis. XOS yield in subsequent hydrolysis by endo-xylanases (from glycoside hydrolase family 10 or 11) was dependent on extraction conditions, and was highest using xylan extracted by 0.5 M NaOH, (42.3%, using Xyn10A from Bacillus halodurans), with xylobiose and xylotriose as main products. The present study shows successful separation of SCB xylan, lignin, and cellulose. High concentration of alkali, resulted in xylan with lower degree of substitution (especially reduced arabinosylation), while high pressure (using PLE), released more lignin than xylan. Enzymatic hydrolysis was more efficient using xylan extracted at lower alkaline strength and less efficient using xylan obtained by PLE and 2 M NaOH, which may be a consequence of polymer aggregation, via remaining lignin interactions.

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