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In this study, a magnesium phosphate whisker (DPM‐H) was synthesized by the acid–base neutralization reaction between magnesium hydroxide and 10‐hydroxy‐9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO‐OH) at 120°C. A new synergistic intumescent flame retardant (IFR) for epoxy resin (EP), which was composed of DPM‐H and ammonium polyphosphate (APP) was thoroughly studied. When the IFR loading was 8%, with the DPM‐H to APP weight ratio at 1:7, the prepared flame‐retardant EP (EPDA‐2) passed the vertical burning tests (UL‐94) V‐0 rating and obtained the limiting oxygen index (LOI) value of 29.3%. Microscale combustion calorimetry (MCC) results showed that the total heat release (THR) of EPDA‐2 reduced by 32.1% compared with pure EP. Meanwhile, the addition of DPM‐H can partially solve the problem of the decrease of the EP mechanical property caused by the addition of APP. Compared with the flame‐retardant EP with the 8% loading of APP, the impact strength of EPDA‐2 increased 152.3%. [ABSTRACT FROM AUTHOR]

Alkaline catalyst is usually used for solvolysis of thermoplastic and thermoset polymers containing ester bonds. However, inorganic catalyst is difficult to remove from products of resin degradation. Here, we reported an efficient and mild degradation method using an organocatalyst, N-methyl-4-piperidinol, in ethylene glycol to degrade methylcyclohexene-1,2-dicarboxylic anhydride (MeTHPA)-cured epoxy resin. N-Methyl-4-piperidinol and ethylene glycol were simultaneously recovered by vacuum distillation. The effects of reaction temperature and catalyst concentration on the reaction rate and kinetics of the degradation reaction were analyzed. The recovery and reuse of ethylene glycol and the catalyst for three cycles were also demonstrated. The degradation products from the epoxy resin were identified by electrospray ionization-mass spectrometry (ESI-MS), and a transesterification mechanism for the degradation of epoxy resin was proposed. [ABSTRACT FROM AUTHOR]

[Display omitted] • Imidazole-based liquid compounds containing different P oxidation states were synthesized for curing EP. • EP-DCPPI and EP-PPOAI show the combined flame-retardant mechanism of gas-phase and condensed-phase flame retardancy. • EP-DCPPI and EP-PPOAI show excellent flame-retardant, mechanical properties and heat resistance. In this work, two phosphorus-containing liquid imidazole compounds with different phosphorus oxidation states (1,1′-(phenylphosphanediyl)bis(1 H -imidazole) (DCPPI) with + 1 valence phosphorus, and imidazole-phenylphosphate (PPOAI) with + 3 valence phosphorus) were designed and synthesized. Both of DCPPI and PPOAI were used as curing agents to obtain intrinsic flame-retardant epoxy resin (EP-DCPPI and EP-PPOAI), in which the imidazole group was used as the curing group of EP, and the phosphorus-containing group was directly connected to the EP crosslinking network. On the one hand, the efficient flame-retardant groups containing + 1 or + 3 valence phosphorus were incorporated into the EP system to obtain excellent flame-retardant properties; on the other hand, the introduction of phenylphosphine or phenoxyphosphine groups in the molecular chain of EP greatly enhanced the interaction between molecular chains, adjusted crosslinking density and endowed EP with excellent tensile strength and toughness. Compared with imidazole cured EP (EP-MZ), the peak heat release rate (PHRR) of EP-15DCPPI and EP-15PPOAI decreased by 70 % and 68 %, and the total heat release rate (THR) decreased by 37 % and 36 %, respectively. Meanwhile, EP-15DCPPI passed UL-94 V-0 rating, and the limiting oxygen index (LOI) reached 36.1 %. EP-15PPOAI passed UL-94 V-1 rating and the LOI reached 29.1 %. The flame-retardant mechanism was analyzed and discussed. Compared with EP-MZ, the dynamic and static mechanical properties of EP-15DCPPI and EP-15PPOAI were enhanced simultaneously, and the glass transition temperature (T g) was obviously increased. [ABSTRACT FROM AUTHOR]

In this work, ammonium phosphomolybdate (AMP) and aluminum diethylphosphinate (ADP) acting as temperature-response microparticles, were incorporated into epoxy resin (EP) together to promote fire safety and dynamic mechanical performance of EP composites at the same time. Both ADP and AMP acted as chemical inertness fillers to enhance the EP matrix at the normal service temperature and processing temperature. When the temperature rose after heating or even burning, both ADP and AMP presented chemical functions. On one hand, AMP exhibited excellent catalytic charring activity and smoke suppression efficiency. On the other hand, the combination between AMP and ADP in the EP/AMP/ADP composites showed excellent synergistic effects in improving the flame retardancy of EP. Compared to the case of EP, the peak heat release rate (PHRR) of EP/AMP/ADP composites (1.2 wt% AMP and 3.6 wt% ADP) was decreased by 54%, the total heat release (THR) was reduced by 25%, and the total smoke production (TSP) was reduced by 25%. Meanwhile, the UL-94 V-0 rating was obtained, and the limiting oxygen index (LOI) of the composite was increased from 26.2 to 31.2%. The mechanism of flame retardancy was analyzed and discussed. In addition, compared with EP, EP/AMP/ADP composites showed a higher dynamic mechanical property without affecting the glass transition temperature. [Display omitted] • The combination of AMP/ADP as temperature-response microparticle shows a synergistic effect in improving fire safety of EP. • The introduction of AMP and ADP changes the degradation process and degradation products of EP. • Both ADP and AMP acted as chemical inertness fillers to enhance EP matrix at the normal service temperature. [ABSTRACT FROM AUTHOR]

Degradation of methyl-1,2-cyclohexanedicarboxylic anhydride (MeHHPA)-cured epoxy resin in subcritical methanol in the presence of potassium hydroxide (KOH) was studied. The degraded products of epoxy resin were first separated using vacuum distillation, extraction and preparative high-performance liquid chromatography (HPLC) and then characterized by HPLC, electrospray ionization mass spectrometry (ESI-MS), 1 H and 13 C nuclear magnetic resonance (NMR). The effects of temperature and KOH on the kinetic behavior of degradation and the product distribution were examined. The temperature for the complete degradation of epoxy resin decreased greatly after adding a small amount of KOH. Transesterification was the dominant mechanism of degradation of epoxy resin. Reaction between KOH and epoxy resin and transetherification mechanism were also proposed. KOH improved the reaction mainly as a catalyst with consumption of methanol but contributed little to the reaction as a reagent. The bending properties of recycled epoxy resin with degraded products obtained at different KOH concentrations were also examined. [ABSTRACT FROM AUTHOR]

It is still a great challenge to develop epoxy resin/glass fabric (EP/GF) composites with well-balanced enhancements on flame retardancy and mechanical properties. Herein, a novel strategy that polyhydric SiO 2 coating assistant to graft organophosphorus (DOPO) onto GF was developed for simultaneously improving flame retardancy and mechanical properties of EP composites. The grafting amount of DOPO could reach to 43.64 wt% via the helpful bridging of polyhydric SiO 2 , so that EP composites displayed excellent flame retardancy with the LOI of 37.2%, the V0 rating on UL-94 and a 63.3% decrease on PHRR in cone calorimeter test. According to the analysis of char morphology and structure, the flame retarded mechanism was mainly ascribed to the enhanced barrier effect of a continuous and intergrow char layer, which was composed of GF@SiO 2 as framework and P-containing condensed carbon as stuffing. Meanwhile, EP composites exhibited outstanding mechanical performances with 35% and 60% increases on tensile strength and impact strength respectively, which resulted from the special molecular structure of GF@SiO 2 - g -DOPO with strong interfacial adhesion with EP chains via hydrogen bond and chemical bond. In summary, this work will be favorable to design multifunctional polymer composites with well-balanced comprehensive performances, and expand their widespread applications in high-end fields. [Display omitted] • A novel polyhydric SiO 2 coating assistant to graft organophosphorus onto GF. • The grafting amount of DOPO could reach to 43.64 wt%. • Excellent flame retardancy with LOI of 37.2%, V0 rating on UL-94 and a 63.3% decrease on PHRR. • Outstanding mechanical performances with 35% and 60% increases on tensile strength and impact strength respectively. • The corresponding enhancement mechanisms on flame retardancy and mechanical performances were revealed. [ABSTRACT FROM AUTHOR]

Abstract: The combination of phenol and potassium hydroxide (KOH) was used to chemically recycle carbon fibre reinforced epoxy resin cured with 4,4′-diaminodiphenylmethane in subcritical water. This combination had a synergistic effect on decomposing this kind of epoxy resin. The main decomposition products from the epoxy resin were identified by means of GC–MS, and a possible free-radical reaction mechanism for the decomposition of epoxy resin is proposed. The recovered carbon fibres were characterized using single fibre tensile tests, scanning electron microscopy and X-ray photoelectron spectroscopy. Compared to virgin carbon fibres after sizing removal, the surface compositions of the recovered carbon fibres had little change and the tensile strength of the recovered carbon fibres was well retained. [Copyright &y& Elsevier]

Abstract: Molybdenum-phenolic resin (Mo-PR) was grafted onto the surface of multi-walled carbon nanotubes (MWCNTs) to obtain modified MWCNTs (CNT-PR). Compared to epoxy resin, epoxy resin/CNT-PR nanocomposites showed the improvements in flame retardancy and mechanical properties. Structural characterization showed that the grafted Mo-PR improved the dispersion of MWCNTs in epoxy resin and enhanced the interfacial interaction between CNT-PR and epoxy resin. On the other hand, the grafted Mo-PR could show high char yield during the process of combustion. Thus the flame retardancy of nanocomposites was improved, especially for the heat release rate and total smoke production. Furthermore, the combination of CNT-PR with melamine dramatically promoted the LOI value and the level of UL-94 rating. [Copyright &y& Elsevier]