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Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides.

ABSTRACT: Increasing attention has been devoted to the design of layered double hydroxide (LDH)-based hybrid materials. In this work, we demonstrate the intercalation by anion exchange process of poly(acrylic acid) (PAA) and three different hydrophilic random copolymers of acrylic acid (AA) and n-butyl acrylate (BA) with molar masses ranging from 2000 to 4200 g mol^-1 synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization, into LDH containing magnesium(II) and aluminium(III) intralayer cations and nitrates as counterions (MgAl-NO₃ LDH). At basic pH, the copolymer chains (macroRAFT agents) carry negative charges which allowed the establishment of electrostatic interactions with the LDH interlayer and their intercalation. The resulting hybrid macroRAFT/LDH materials displayed an expanded interlamellar domain compared to pristine MgAl-NO₃ LDH from 1.36 nm to 2.33 nm. Depending on the nature of the units involved into the macroRAFT copolymer (only AA or AA and BA), the intercalation led to monolayer or bilayer arrangements within the interlayer space. The macroRAFT intercalation and the molecular structure of the hybrid phases were further characterized by Fourier transform infrared (FTIR) and solid-state ¹³C, ¹H and ²⁷Al nuclear magnetic resonance (NMR) spectroscopies to get a better description of the local structure.

SUBMITTER: Kostadinova D

PROVIDER: S-EPMC5238628 | biostudies-literature | 2016

REPOSITORIES: biostudies-literature

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Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides.

Kostadinova Dessislava D Cenacchi Pereira Ana A Lansalot Muriel M D'Agosto Franck F Bourgeat-Lami Elodie E Leroux Fabrice F Taviot-Guého Christine C Cadars Sylvian S Prevot Vanessa V

Beilstein journal of nanotechnology 20161215

Increasing attention has been devoted to the design of layered double hydroxide (LDH)-based hybrid materials. In this work, we demonstrate the intercalation by anion exchange process of poly(acrylic acid) (PAA) and three different hydrophilic random copolymers of acrylic acid (AA) and <i>n</i>-butyl acrylate (BA) with molar masses ranging from 2000 to 4200 g mol<sup>-1</sup> synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization, into LDH containing magnesium(II) a ...[more]

PMID: 28144548

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Project description:The development of halogen-free flame retardants as environmentally friendly and renewable materials for heat and fire-resistant applications in the field of electronics is important to ensure safety measures. In this regard, we have proposed a simple and halogen-free strategy for the synthesis of flame retardant LDH-PN materials to decrease the fire hazards of epoxy resin (EP), via a co-precipitation reaction between Mg(NO3)2 and Al(NO3)3 and the subsequent incorporation of different cyclotriphosphazene (PN) carboxylate anions. The cyclotriphosphazene-based di, tetra and hexacarboxylate-intercalated layered double hydroxides are designated as LDH-PN-DC, LDH-PN-TC and LDH-PN-HC, respectively. Furthermore, the intercalation of cyclotriphosphazene carboxylate anions into the LDH layers was confirmed by PXRD, FT-IR, TGA, solid-state 31P NMR, nitrogen adsorption and desorption analysis (BET), HR-SEM and XPS. Evaluation of the flame retardant (vertical burning test and limiting oxygen index) properties was demonstrated by formulating the LDH-PN materials with epoxy resin (EP) in different ratios coated on wood substrates to achieve the desired behaviour of the EP/LDH-PN composites. Structure-property analysis reveals that EP/LDH-PN-TC-20 wt% and EP/LDH-PN-HC-20 wt% achieved a V 0 rating in the UL-94 V test and achieved higher LOI values (27.7 vol% for EP/LDH-PN-TC-20 wt% and 29 vol% for EP/LDH-PN-HC-20 wt%) compared to the epoxy-coated wood substrate (23.2 vol%), whereas EP/LDH-PN-DC failed in the vertical burning test for various weight percentages of LDH-PN-DC from 5 wt% to 20 wt% in the composites, with a lower LOI value of 22.1 vol%. Excellent flame retardancy was observed for EP/LDH-PN-TC and EP/LDH-PN-HC due to the presence of more binding sites of carboxylate anions in the LDH layers and less or no spiro groups in cyclotriphosphazene compared to that in EP/LDH-PN-DC. In addition, the synergistic flame retardant effect of the combination of LDH and cyclotriphosphazene on the epoxy resin composites remains very effective in creating a non-volatile protective film on the surface of the wood substrate to shelter it from air, absorb the heat and increase the ignition time, which prevents the supply of oxygen during the combustion process. The results of this study show that the proposed strategy for designing flame-retardant properties represents the state-of-the-art, competent coating of inorganic materials for the protection and functionalization of wood substrates.

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Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides.

Publications

Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides.

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