scholarly journals The Use of the ATD Technique to Measure the Gelation Time of Epoxy Resins

Materials ◽  
2021 ◽  
Vol 14 (20) ◽  
pp. 6022
Author(s):  
Jakub Smoleń ◽  
Piotr Olesik ◽  
Paweł Gradoń ◽  
Mateusz Chudy ◽  
Bogusław Mendala ◽  
...  

In this paper, we investigated the thermodynamics of the resin curing process, when it was a part of composition with graphite powder and cut carbon fibers, to precisely determine the time and temperature of gelation. The material for the research is a set of commercial epoxy resins with a gelation time not exceeding 100 min. The curing process was characterized for the neat resins and for resins with 10% by weight of flake graphite and cut carbon fibers. The results recorded in the analysis of temperature derivative (ATD) method unequivocally showed that the largest first derivative registered during the test is the gel point of the resin. The innovative approach to measuring the gelation time of resins facilitates the measurements while ensuring the stability of the curing process compared to the normative tests that introduce mechanical interaction. In addition, it was found during the research that the introduction of 10% by weight of carbon particles in the form of graphite and cut carbon fibers rather shortens the gelation time and lowers the temperature peak due to the effective absorption and storage of heat from the cross-linking system. The inhibiting (or accelerating) action of fillers is probably dependent on chemical activity of the cross-linking system.

Author(s):  
Istebreq A. Saeedi ◽  
Sunny Chaudhary ◽  
Thomas Andritsch ◽  
Alun S. Vaughan

AbstractReactive molecular additives have often been employed to tailor the mechanical properties of epoxy resins. In addition, several studies have reported improved electrical properties in such systems, where the network architecture and included function groups have been modified through the use of so-called functional network modifier (FNM) molecules. The study reported here set out to investigate the effect of a glycidyl polyhedral oligomeric silsesquioxane (GPOSS) FNM on the cross-linking reactions, glass transition, breakdown strength and dielectric properties of an amine-cured epoxy resin system. Since many previous studies have considered POSS to act as an inorganic filler, a key aim was to consider the impact of GPOSS addition on the stoichiometry of curing. Fourier transform infrared spectroscopy revealed significant changes in the cross-linking reactions that occur if appropriate stoichiometric compensation is not made for the additional epoxide groups present on the GPOSS. These changes, in concert with the direct effect of the GPOSS itself, influence the glass transition temperature, dielectric breakdown behaviour and dielectric response of the system. Specifically, the work shows that the inclusion of GPOSS can result in beneficial changes in electrical properties, but that these gains are easily lost if consequential changes in the matrix polymer are not appropriately counteracted. Nevertheless, if the system is appropriately optimized, materials with pronounced improvements in technologically important characteristics can be designed.


2019 ◽  
Vol 138 (6) ◽  
pp. 4349-4358 ◽  
Author(s):  
K. Fila ◽  
M. Gargol ◽  
M. Goliszek ◽  
B. Podkościelna

Abstract The aim of this study was the synthesis of three different epoxy compounds based on naphthalene-2,7-diol (2,7-NAF.EP, 2,7-NAF.WEP, 2,7-NAF.P.EP) and then their cross-linking by triethylenetetramine (TETA). All epoxides were prepared by the reaction of naphthalene-2,7-diol with epichlorohydrin but under different conditions and with other catalysts. The structures of the obtained compounds before and after the cross-linking reactions were confirmed by the attenuated total reflectance Fourier transform infrared spectroscopy (ATR/FT-IR). The ATR/FT-IR spectra of cross-linked compounds show disappearance of the C–O–C bands (about 915 cm−1) derived from the epoxy groups. DSC and TG/DTG measurements indicated that the obtained materials possess good thermal resistance; they are stable up to about 250 °C. The hardness of the cross-linked products was determined using the Shore D method. The highest value of hardness was obtained for the 2,7-NAF.EP-POL. Additionally, the UV–Vis absorption spectra of the obtained polymers were registered and evaluated.


1985 ◽  
Vol 5 (12) ◽  
pp. 1041-1051 ◽  
Author(s):  
Joseph M. Wu ◽  
Stanley J. Wertheimer ◽  
Behruz Eslami ◽  
Joanne C. Figuereido ◽  
Biswendu B. Goswami

Rabbit reticulocyte lysates, gel filtered on Sephadex G-25 with or without ATP (or its analogs), were preincubated at 37°C and their subsequent binding to p3A4,3′-[32P]pCp was studied. Lysates filtered without ATP or in the presence of 0.1 mM 8-bromo-ATP, 1,N6-etheno-ATP, or ITP showed a time-dependent decrease in binding activity. This decrease was completely prevented when lysates were filtered with 0.1 mM ATP, 2′-deoxy-ATP, β-γ-methylene-ATP, or ATP-γ-S. The stability of binding provided by ATP or 2′-deoxy-ATP analogs corresponds to a more active 2–5A dependent endonucleolytic (RNAase L) activity based on studies using [3H] viral mRNA. Chromatography on heparin-agarose showed that ATP-supplemented gel-filtered reticulocyte lysates had a different p3A4,3′-[32P]pCp binding activity elution-profile than lysates gel-filtered in the absence of ATP. Covalent cross-linking of periodate-oxidized p3A4,3′-[32P]pC to gelfiltered lysates, preincubated at 0°C or 37°C for 30 min, showed the following results: (1) all lysates gave a major cross-linking of the radioactive ligand to an 80 000 dalton polypeptide, regardless of the temperature of preincubation, (2) Iysates gel-filtered without ATP, with 0.1 mM ITP, or β-γ-methylene-ATP, showed a significant reduction in the cross-linking of the 80 000 dalton protein, after preincubation at 37°C for 30 min. This decrease was accompanied by an increase in the labeling of two smaller polypeptides.


NANO ◽  
2021 ◽  
pp. 2150008
Author(s):  
Hongwei Liu ◽  
Jinhua Liu ◽  
Jun Li ◽  
Zhanchao Liu ◽  
Weifu Wu ◽  
...  

An excellent novel laminar and hierarchical polyethyleneimine cross-linked graphene oxide/titanium dioxide (GO–TiO2–PEI) membrane was successfully prepared by vacuum filtration technology using polyethyleneimine (PEI) as the cross-linking agent and a GO–TiO2 nanocomposite as the substrate. The resultant membrane (GO–TiO2–PEI) displayed a favorable antifouling performance with bovine serum albumin (BSA) and showed good hydrophilicity and wettability, with a static water contact angle of 13.2∘. The stability of the GO–TiO2–PEI membrane in aqueous solution obviously improved with the cross-linking of PEI compared with that of the GO and GO–TiO2 membranes. The GO–TiO2–PEI membrane also exhibited a satisfactory water flux of 48.6[Formula: see text]L m[Formula: see text] h[Formula: see text] bar[Formula: see text]. The GO–TiO2–PEI membrane exhibited a good performance for effectively separating different dyes including methylene blue (MB), rhodamine B (RB), methyl orange (MO), sunset yellow (SY), new coccine (NC) and amaranth. All the above results suggested that the GO–TiO2–PEI membrane could be used as an excellent stable hydrophilic membrane for efficiently separating dyes from aqueous solution.


1995 ◽  
Vol 7 (2) ◽  
pp. 219-236 ◽  
Author(s):  
K A Kozielski ◽  
N C Billingham ◽  
G A George ◽  
D C L Greenfield ◽  
J M Barton

The cross-linking reactions of 4,4'-diaminodiphenyl sulphone (DDS) with stoichiometric quantities of glycidyl ether- or tetraglycidyl amine-based epoxy resins were monitored using chemiluminescence (CL) and rheometry. It was found that, when a sample was cured isothermally in air, the CL profile increased to a maximum, then decreased again. The maximum was found to correspond well with the gel time (tgel), as measured by rheometry. This observation is discussed in relation to the chemical reactions occurring within the material and the physical state of the matrix. The effect of impurities in DDS on the gel time of these epoxy resins is reported.


Holzforschung ◽  
2011 ◽  
Vol 65 (3) ◽  
Author(s):  
Lars Passauer ◽  
Klaus Fischer ◽  
Falk Liebner

Abstract Highly swellable, mechanically stable hydrogels were obtained by cross-linking different technical lignins with poly(ethylene) glycol diglycidyl ether (PEGDGE). The gelation time and the properties of the products can be controlled by the extent of pre-oxidation and the cross-linking conditions, namely the dynamic viscosity η*, storage and loss modulus (G′; G″), and loss factor tan δ. The highest free swelling capacities (FSC) of up to 50 g water per g xerogel were obtained from pre-oxidized pine kraft lignin Indulin® AT and spruce organosolv lignin. Dynamic rheological measurements confirmed the typical rheological behaviour of gel structures, i.e. a linear decrease of dynamic viscosity about three orders of magnitude within a frequency range of 0.08 and 20 s-1. The results furthermore revealed a good mechanical sturdiness of the cross-linked lignin hydrogels. Sandy soils supplemented with small quantities of the hydrogels were found to feature a significantly increased plant-available water content. Based on the observed effects, oligo(oxyethylene) lignins are promising materials with respect to a prolonged water retention in soils.


2001 ◽  
Vol 34 (13) ◽  
pp. 4526-4533 ◽  
Author(s):  
Bor-Sen Chiou ◽  
Srinivasa R. Raghavan ◽  
Saad A. Khan

2017 ◽  
Vol 748 ◽  
pp. 39-44 ◽  
Author(s):  
Stefano Merighi ◽  
Emanuele Maccaferri ◽  
Juri Belcari ◽  
Andrea Zucchelli ◽  
Tiziana Benelli ◽  
...  

Interaction between poly (m-phenylene isophtalamide) (PMIA) electrospun nanofibers and commercial epoxy resin precursor during the cross-linking process was investigated, in order to use such polyaramidic nanofibers for composite materials reinforcement. Hence nanofibrous PMIA mats were produced via electrospinning technique to be used for the functional modification of the epoxy matrix composite properties. When adding such fibers to an epoxy resin precursor, it was observed a strong influence on the kinetics of its curing process. The final results, however, demonstrates that boosting the reaction condition (raising the temperature and the reaction time) the curing is pushed to completion, indicating that the cross-linking process of the resin is just delayed and not completely hampered. It will be therefore necessary to rethink the composite cure cycle when PMIA nanofibers are added to the composite material, in order to attain significant improvement of the final composite performance.


2021 ◽  
Vol 25 (1) ◽  
pp. 49-52
Author(s):  
Aleksandra Kłos-Witkowska ◽  
Vasyl Martsenyuk

In this study, the stability of the receptor layer component of a biosensor after addition of gold nanoparticles was investigated. Accelerated conformational changes under the influence of Au were demonstrated. The relative percentage changes over time between the pure protein and the Au doped protein were calculated. It was shown that these changes are greater with time and exceed 20 % in the last days of the experiment.


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