Preparation, thermal properties, and flame retardance of epoxy–silica hybrid resins

Liu, Ying‐Ling; Wu, Chuan‐Shao; Chiu, Yie‐Shun; Ho, Wen-Hsuan

doi:10.1002/pola.10778

Cited by 162 publications

(103 citation statements)

References 34 publications

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“…16 Through the reaction between P-H group and oxirane group, DOPO was incorporated into ES to synthesize PES, a kind of DOPO-containing epoxy-siloxane ( Figure 1). Seen from the FT-IR spectrums of PES and ES (Figure 4), no absorption peak at 2384 cm À1 (P-H) was observed in PES curve, and the appearance of the peak at 3430 cm À1 (-OH), which was an indication of the occurrence of the reaction.…”

Section: Synthesis and Characterization Of Pesmentioning

confidence: 99%

Studies on the Thermal Properties and Flame Retardancy of Epoxy Resins Modified with Polysiloxane Containing Organophosphorus and Epoxide Groups

Hou

Liu

et al. 2007

Polym J

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ABSTRACT:A novel epoxy resin modifier, phosphorus-containing epoxide siloxane (PES) with pendant epoxide and cyclic phosphorus groups on the side chain of the polysiloxane backbone, was synthesized by the ring-opening reaction of epoxy-siloxane with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). PES was characterized by 1 H NMR and FT-IR measurements, and then it was employed to modify an epoxy resin at various ratios via prereaction with 4, 4 0 -diaminodiphenyl-methane (DDM) as curing agent. In order to compare with the epoxy resins modified with PES, DOPO-containing epoxy resins also cured under the same conditions. The thermal, thermomechanical, and flame-retardant properties of all cured polymers were investigated by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), thermogravimetric analysis (TGA), the limited oxygen index (LOI) and cone calorimetry. The results showed that the epoxy resins modified with PES exhibited much better thermal properties and flame retardancy than the DOPO-containing epoxy resins at the same phosphorus content and the neat epoxy resin. In recent years, epoxy resins have been widely used in coatings, adhesives, aerospace and electronic industries, especially in microelectronic field. However, with the rapid development of electronic technology, the heat resistance and flame retardancy of conventional epoxy resins couldn't meet the requirements of these applications. 1,2 Much work has been done in an attempt to make epoxy resin more flame retardancy and great progress has been achieved so far. [3][4][5][6][7][8][9][10] At present, with the consideration of avoiding the generation of toxic and halogenated gases, the trend is toward using environment-friendly flame retardant to modify the epoxy resins. One example is the use of organophosphorus, which shows evident effectiveness as a flame retardant. [4][5][6][7][8] However, this increase in flame retardancy is always accompanied by a decrease in the initial decomposition temperature, which makes the modified epoxy resins unfit for those applications requiring critical thermal stability. Moreover, due to the limit from chemical structures in molecular design during the introduction of phosphorus, the low crosslink density of the cured epoxy resin often decreases T g of the epoxy resin. 9,10 According to a previous report, 11 the flame retardancy of phosphorus could be improved if providing an environment to reduce the thermal oxidation of phosphorus char at the high temperature region. Organosiloxanes possess many properties, including hydrophobic property, non-flammability, excellent thermo-oxidative stability and electronic property, which can compensate for the disadvantages of phosphorus flame retardant. Thus, organosiloxanes would be one of choices for enhancing the flame retardancy and heat resistance. [12][13][14] In this paper, a novel modifier for epoxy resins, epoxy oligomer containing organophosphorus and organosilicon, was synthesized by the reaction of methylhydrosiloxane-dimethylsil...

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Section: Synthesis and Characterization Of Pesmentioning

confidence: 99%

Studies on the Thermal Properties and Flame Retardancy of Epoxy Resins Modified with Polysiloxane Containing Organophosphorus and Epoxide Groups

Hou

Liu

et al. 2007

Polym J

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“…The weight loss of the pure UP below 300 °С is small and the main loss weight occurs in the range of 300~490 °С. Compared with that of the pure UP, the weight loss of UP-DIs increases below 300 °С, which is maybe due to the decomposition of the DOPO group containing the P-O band of low bond energy [12]. The weight loss of UP-DI20 attains 12% below 300 °С.…”

Section: Tg Analysis In Nitrogenmentioning

confidence: 92%

“…However, the UPclay nanocomposites are opaque and cannot satisfy the increasing requirements for transparent flame-retarded application of thermosetting resin materials in advanced electronics [11]. Additionally, polymer/SiO 2 nanocomposites by a sol-gel process exhibit to some degree flame-retardance effect by the formation of the carbonaceoussilicate char building up on the polymer surface during burning [12][13][14]. Generally, the poor compatibility between organic polymer and silica gel results in aggregation of silica networks in an organic polymer matrix during the formation of the silica gel, and then the appearance of the obtained composite materials is turbid or phase separated.…”

Section: Introductionmentioning

confidence: 99%

Flame retardance and thermal properties of a novel phosphorus-containing unsaturated polyester resin/SiO2 hybrid nanocomposite

et al. 2009

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A novel phosphorus-containing unsaturated polyester resin/SiO 2 hybrid nanocomposite was prepared from the in-situ curing of unsaturated polyester resin (UP) and triethoxysilane (DI) which was synthesized from the nucleophilic addition reaction of 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) and 3-(trieoxysilyl) isocyanate(icteos). The formation of unsaturated polyester resin/SiO 2 hybrid nanocomposite (UP-DI) was confirmed by infrared spectra (FTIR) and scanning electron microscopy (SEM). With the increase of DI contents, the limiting oxygen index (LOI) value of the cured UP-DIs was raised from 19 to 29, suggesting a significant improvement in flame retardance. The improved flame retardance could also be revealed by the variations of weight and morphology of char residues. Thermogravimetric analysis (TGA) both in air and in nitrogen was used to estimate mechanism of thermal degradation and activation energy (E a ) of different degree of conversion (α) was calculated by Ozawa's method. The UP-DI containing 10%DI (UP-DI10) had higher E a than the pure UP as α>5% because the degradation mechanism was altered by the incorporation of DI.

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“…It can be observed that the short stage of degradation for neat and modified resin occurred around 245 and 235 °C, respectively, with an approximately 7% weight loss. This fact is attributed to the presence of impurities 11,37 . In both polymeric systems, the main degradation takes place above 390 °C, owing to the thermal degradation of epoxy network.…”

Section: Thermogravimetric Analysismentioning

confidence: 99%

Development and characterization of composite materials for production of composite risers by filament winding

2011

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Industry has been challenged to provide riser systems which are more cost effective and which can fill the technology gaps with respect to water depth, riser diameter and high temperatures left open by flexibles, steel catenary risers (SCRs) and hybrid risers. Composite materials present advantages over conventional steel risers because composite materials are lighter, more fatigue and corrosion resistant, better thermal insulators and can be designed for improving the structural and mechanical response. This paper contains a study of the toughening mechanism of an epoxy resin under rubber addition by means of fractographic analysis and its relation with the fracture process and increase of strength of a composite riser employing this polymeric matrix. Initially, an epoxy resin system was toughened by rubber CTBN addition (10 wt. (%)) as a way of improving the flexibility of future risers. Mechanical and thermal analyses were carried out for characterizing the polymeric systems. Later, composite tubes were prepared and mechanically characterized. The influence of matrix toughening on the mechanical behavior of the tubes was also studied. Split-disk tests were used to determine the hoop tensile strength of these specimens. The results indicate that the matrix plays an important role in composite fracture processes. The adding rubber to the polymeric matrix promoted a simultaneous increase of stress and elongation at fracture of the tubes manufactured herein, which is not often reported. These results, probably, is function of better adhesion between fibers and polymeric matrix observed in the CTBN-modified composite rings, which was evidenced in the fractografic analysis by SEM after the split-disk tests.

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Preparation, thermal properties, and flame retardance of epoxy–silica hybrid resins

Cited by 162 publications

References 34 publications

Studies on the Thermal Properties and Flame Retardancy of Epoxy Resins Modified with Polysiloxane Containing Organophosphorus and Epoxide Groups

Studies on the Thermal Properties and Flame Retardancy of Epoxy Resins Modified with Polysiloxane Containing Organophosphorus and Epoxide Groups

Flame retardance and thermal properties of a novel phosphorus-containing unsaturated polyester resin/SiO2 hybrid nanocomposite

Development and characterization of composite materials for production of composite risers by filament winding

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