Synthesis, structural, and thermal characterization of a new binuclear copper(II) chelate complex bearing an amine-hardener for epoxy resins

Lavrenyuk, Helen; Mykhalichko, Oleg; Zarychta, Bartosz; Olijnyk, Volodymyr; Mykhalichko, B. M.

doi:10.1080/00958972.2016.1212340

Cited by 13 publications

(10 citation statements)

References 24 publications

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“…All reflections from crystal lattice (see Figure ) have been indexed; unit cell parameters have been refined ( a = 7.6504(4), b = 7.1991(3), c = 22.088(1) Å, β = 98.493(5)°, space group P 2 1 / c ). Hence, the DETA ‐CuCO 3 is a dehydrated analog of the [{C u ( DETA )(H 2 O)(μ‐CO 3 )} 2 ] ⋅ 6H 2 O chelate complex whose crystal structure has been studied earlier …”

Section: Results and Disscussionmentioning

confidence: 99%

“…As shown in Figure A, the TGA curve of the thermal decomposition of the originally hydrated DETA ‐CuCO 3 complex is represented by 4 sections. The first section involves the temperature range from 20°C to 154°C.…”

Section: Results and Disscussionmentioning

confidence: 99%

“…The samples of the CuCO 3 ‐containing epoxy‐amine polymer, where the molar ratio DGEBA : DETA :CuCO 3 is 5:2:2, can also be obtained on the basis of the [{Cu( DETA )(H 2 O)(μ‐CO 3 )}]⋅6H 2 O chelate complex whose synthesis was described in detail in Lavrenyuk et al According to the alternative method of obtaining the DGEBA / DETA ‐CuCO 3 (12), the DETA ‐CuCO 3 polycrystalline powder (22 g, 0.1 mol) prepared by dehydration of the [{Cu( DETA )(H 2 O)(μ‐CO 3 )}]⋅6H 2 O was added to DGEBA (100 g). All further manipulations with the reaction mixture were performed in accordance with above‐said procedures of preparing the CuCO 3 ‐containing epoxy‐amine polymers.…”

Section: Methodsmentioning

confidence: 99%

“…The indexing of the XRPD pattern was fulfilled automatically by means of the method described in Louër and Louër, using DICVOL91 software package . The structure model was taken from single crystal data of the [{Cu( DETA )(H 2 O)(μ‐CO 3 )}]⋅6H 2 O chelate complex …”

Section: Methodsmentioning

confidence: 99%

“…Proceeding further in influence study of the cupric salts onto combustibility of the epoxy‐amine polymers, we have replaced the copper(II) sulfate by the copper(II) carbonate in above system. As a result, the chelate complex denoted as DETA ‐CuCO 3 that further was used as a fire retardant hardener of epoxy resins have been educed out of the DETA ‐ DGEBA ‐CuCO 3 system.…”

Section: Introductionmentioning

confidence: 99%

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Metal‐coordinated epoxy polymers with suppressed combustibility. Preparation technology, thermal degradation, and combustibility test of new epoxy‐amine polymers containing the curing agent with chelated copper(II) carbonate

Lavrenyuk

Кочубей

Mykhalichko³

et al. 2017

Fire and Materials

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Summary The diethylenetriamine chelate complex of copper(II) carbonate—DETA‐CuCO3 (a fire retardant hardener of epoxy resins)—and the CuCO3‐containing epoxy‐amine polymers—DGEBA/DETA‐CuCO3(6), DGEBA/DETA‐CuCO3(12), DGEBA/DETA‐CuCO3(40), and DGEBA/DETA‐CuCO3(80) with suppressed combustibility—have been obtained in the DETA‐DGEBA‐CuCO3 system (DETA and DGEBA are diethylenetriamine and bisphenol A diglycidyl ether, respectively). The DETA‐CuCO3 chelate complex was characterized by X‐ray powder diffraction, infrared spectra, and thermal analysis. The thermal gravimetric analysis results have revealed that thermal destruction of DETA‐CuCO3 was finished at 400°С, and the maximal temperature of the combustion gases amounted to 520°С. The thermal behavior and combustibility of the CuCO3‐containing epoxy‐amine polymers were studied using thermal analysis and “Ceramic tube” (CT) method. Thermal gravimetric analysis confirms that incorporation of the DETA‐CuCO3 into DGEBA appreciably heightens the thermal stability and antiflammability of the CuCO3‐containing epoxy‐amine polymers. Results of CT measurement reveal that maximal temperature of the combustion gases under burning of the DGEBA/DETA‐CuCO3(12) sample in comparison with unmodified epoxy‐amine polymer (DGEBA/DETA) is lowered on 219°С and the loss of weight is decreased on 20.5 wt%. According to ASTM 635‐14, ASTM D2863‐13, and ASTM D1929‐16, the flame propagation rate, limiting oxygen index, and temperatures of ignition and self‐ignition have been measured for the elaborated polymer samples.

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Section: Results and Disscussionmentioning

confidence: 99%

Section: Results and Disscussionmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Metal‐coordinated epoxy polymers with suppressed combustibility. Preparation technology, thermal degradation, and combustibility test of new epoxy‐amine polymers containing the curing agent with chelated copper(II) carbonate

Lavrenyuk

Кочубей

Mykhalichko³

et al. 2017

Fire and Materials

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New copper(II)‐coordinated epoxy‐amine polymers with flame‐self‐extinguishment properties: Elaboration, combustibility testing, and flame propagation rate measuring

et al. 2020

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Summary In the DGEBA ‐ pepa ‐ CuSiF6 system (DGEBA is diglycidyl ether of bisphenol A; pepa is polyethylenepolyamine containing ethylenediamine (eda) and diethylenetriamine (deta)), a new flame retardant‐hardener for epoxy resins in the form of a chelate complex [Cu(eda)(deta)]SiF6 was synthesized and incorporated into the DGEBA to obtain a number of CuSiF6‐containing epoxy‐amine polymers with reduced combustibility and flame‐self‐extinguishment properties. The resulting samples of the DGEBA/pepa‐CuSiF6(I‐V) were characterized using FTIR spectra, combustibility, and flammability tests and the smoke formation factor measurements. The combustibility of the polymer samples were investigated using “Ceramic tube” (CT) method. Results of CT measurement reveal that maximal temperature of gaseous products of combustion for modified epoxy‐amine polymers in comparison with the unmodified epoxy appreciably goes down and weight loss lessen. The flammability of the samples was evaluated by means of UL94 BH and UL94 BV methods. The burning rate of the DGEBA/pepa‐CuSiF6(III) and DGEBA/pepa‐CuSiF6(IV) polymers containing 44 and 66 weight fractions of CuSiF6, respectively, is dramatically reduced compared to that for unmodified epoxy (these samples do not support flame propagation). The rburn. Values for the unmodified epoxy‐amine sample (DGEBA/pepa) is 25.13 mm·min−1.

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Elaboration, thermogravimetric analysis, and fire testing of a new type of wood‐sawdust composite materials based on epoxy–amine polymers modified with copper(II) hexafluorosilicate

2021

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SUMMARY The study reports the development of a new type of wood‐sawdust (WS) composite based on CuSiF6‐modified epoxy–amine polymers (EAPs) with reduced combustibility. The thermo‐oxidative behavior of the obtained WS/EAP–CuSiF6 and WS/EAP specimens was studied using the complex thermal analysis. Thermal analysis data show that incorporating CuSiF6 (flame retardant) into WS/EAP increases the thermal oxidation resistance of WS/EAP–CuSiF6. It is shown that for WS/EAP–CuSiF6 and WS/EAP, thermo‐oxidative destruction ends at 571°C and 625°C, and the maximum temperature of this exothermic process is 435°C and 499°C, respectively. The combustibility of WS/EAP–CuSiF6 and WS/EAP was studied by the “ceramic tube” (CT) method. The CT results obtained demonstrate impressive differences in the combustibility of these two composites; the maximum temperature of gaseous combustion products for WS/EAP–CuSiF6 is 265°C, and for WS/EAP, it is 910°C. Flammability tests for WS/EAP–CuSiF6 and WS/EAP were carried out in accordance with ASTM D635‐18 and ASTM D3801‐19a. According to the results of vertical burning tests, the WS/EAP–CuSiF6 composite material was classified as V‐0.

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Synthesis, structural, and thermal characterization of a new binuclear copper(II) chelate complex bearing an amine-hardener for epoxy resins

Cited by 13 publications

References 24 publications

Metal‐coordinated epoxy polymers with suppressed combustibility. Preparation technology, thermal degradation, and combustibility test of new epoxy‐amine polymers containing the curing agent with chelated copper(II) carbonate

Metal‐coordinated epoxy polymers with suppressed combustibility. Preparation technology, thermal degradation, and combustibility test of new epoxy‐amine polymers containing the curing agent with chelated copper(II) carbonate

New copper(II)‐coordinated epoxy‐amine polymers with flame‐self‐extinguishment properties: Elaboration, combustibility testing, and flame propagation rate measuring

Elaboration, thermogravimetric analysis, and fire testing of a new type of wood‐sawdust composite materials based on epoxy–amine polymers modified with copper(II) hexafluorosilicate

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