scholarly journals Preparation, Characterization, Thermal, and Flame-Retardant Properties of Green Silicon-Containing Epoxy/Functionalized Graphene Nanosheets Composites

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Ming-Yuan Shen ◽  
Chen-Feng Kuan ◽  
Hsu-Chiang Kuan ◽  
Chia-Hsun Chen ◽  
Jia-Hong Wang ◽  
...  

In this investigation, silane was grafted onto the surface of graphene nanosheets (GNSs) through free radical reactions, to form Si-O-Et functional groups that can undergo the sol-gel reaction. To improve the compatibility between the polymer matrix and the fillers, epoxy monomer was modified using a silane coupling agent; then, the functionalized GNSs were added to the modified epoxy to improve the thermal stability and strengthen the flame-retardant character of the composites. High-resolution X-ray photoelectron spectrometry reveals that when the double bonds in VTES are grafted to the surfaces of GNSs. Solid-state 29Si nuclear magnetic resonance presents that the distribution of the signal associated with the T3structure is wide and significant, indicating that the functionalization reaction of the silicone in the modified epoxy and VTES-GNSs increases the network-like character of the structures. Thermal gravimetric analysis, the integral procedure decomposition temperature, and limiting oxygen index demonstrate that the GNSs composites that contained silicon had a higher thermal stability and stronger flame-retardant character than pure epoxy. The dynamic storage modulus of all of the m-GNSs containing composites was significantly higher than that of the control epoxy, and the modulus of the composites increased with the concentration of m-GNSs.

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 720 ◽  
Author(s):  
Chen ◽  
Chiang

The NCO functional group of 3-isocyanatoproplytriethoxysilane (IPTS) and the OH functional group of 10-(2,5-dihydroxyphenyl)-10H-9-oxa-10-phospha-phenantbrene-10-oxide (DOPO-BQ) were used to conduct an addition reaction. Following completion of the reaction, triglycidyl isocyanurate (TGIC) was introduced to conduct a ring-opening reaction. Subsequently, a sol–gel method was used to initiate a hydrolysis–condensation reaction on TGIC–IPTS–DOPO-BQ to form a hyperbranched nitrogen–phosphorous–silicon (HBNPSi) flame retardant. This flame retardant was incorporated into a polyurethane (PU) matrix to prepare a hybrid material. Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), limiting oxygen index (LOI), UV-VIS spectrophotometry, and Raman analysis were conducted to characterize the structure and analyze the transparency, thermal stability, flame retardancy, and residual char to understand the flame retardant mechanism of the prepared hybrid material. After the flame retardant was added, the maximum degradation rate decreased from −36 to −17 wt.%/min, the integral procedural decomposition temperature (IPDT) increased from 348 to 488 °C, and the char yield increased from 0.7 to 8.1 wt.%. The aforementioned results verified that the thermal stability of PU can be improved after adding HBNPSi. The LOI analysis indicated that the pristine PU was flammable because the LOI of pristine PU was only 19. When the content of added HBNPSi was 40%, the LOI value was 26; thus the PU hybrid became nonflammable.


2014 ◽  
Vol 67 (11) ◽  
pp. 1688 ◽  
Author(s):  
Jinyun Zheng ◽  
Yujian Yu ◽  
Lulu Zhang ◽  
Xiaomin Zhen ◽  
Yufen Zhao

Two novel types of phosphate derivatives of phosphaphenanthrene with a high phosphorus content were prepared by phosphorylation reaction between either 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)-methanol (ODOPM) or 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)-1,4-benzenediol (ODOPB) and dialkyl phosphoryl chloride. The structures of all compounds were characterised by 1H NMR, 13C NMR, 31P NMR, Fourier transform infrared spectroscopy, and high-resolution mass spectrometry. The thermal stability of representative compounds was determined by thermal gravimetric analysis and differential scanning calorimetry. The results showed that the compounds have excellent resistance to oxidation, high thermal stability with an onset decomposition temperature above 200°C, and a high char yield over 25 %, owing to the high P content. The representative compound was added to conventional electrolytes of lithium-ion batteries as flame retardant additive, and the self-extinguishing time and ionic conductivity were measured. The result showed that the compounds have effective flame retardant properties.


Polymers ◽  
2021 ◽  
Vol 13 (17) ◽  
pp. 2977
Author(s):  
Shang-Hao Liu ◽  
Cing-Yu Ke ◽  
Chin-Lung Chiang

In the study, agricultural waste bagasse was used as a bio-based flame retardant for reducing the flammability of epoxy. Specifically, an interpenetrating network (IPN) was formed through a ring opening reaction between the hydroxyl functional group of bagasse and the epoxy group of triglycidyl isocyanurate (TGIC), forming Bagasse@TGIC. Next, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) was mixed with Bagasse@TGIC, inducing a reaction between the active hydrogen of DOPO and the epoxy group of TGIC, ultimately forming Bagasse@TGIC@DOPO with an IPN structure. Finally, the novel flame retardant was added to epoxy to create a composite. The integral procedural decomposition temperature (IPDT) of pure epoxy is 619 °C; after the introduction of the 30 wt% flame retardant, the IPDT of the resultant composite material increased to 799 °C, greatly increasing the thermal stability by 29%. After the addition of the Bagasse@TGIC@DOPO flame retardant, the limiting oxygen index increased from 21% for the pure epoxy to 29% for the composite, and the UL-94 rating improved from failing rating for the pure epoxy and V-0 rating for the composite. The Raman spectrum indicated that the addition of Bagasse@TGIC@DOPO IPN substantially increased the biochar yield during the burning process, increasing thermal stability. These results confirmed that the epoxy/Bagasse@TGIC@DOPO composite had substantial flame retarding effects.


Polymers ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 1575 ◽  
Author(s):  
Peng Xu ◽  
Peiyuan Shao ◽  
Qing Zhang ◽  
Wen Cheng ◽  
Zichao Li ◽  
...  

A novel flame-retardant composite material based on zinc alginate (ZnAlg) and nano-cuprous oxide (Cu2O) was prepared through a simple, eco-friendly freeze-drying process and a sol-gel method. The composites were characterized and their combustion and flammability behavior were tested. The composites had high thermal stability and achieved nearly non-flammability with a limiting oxygen index (LOI) of 58. The results show remarkable improvement of flame-retardant properties in the ZnAlg/Cu2O composites, compared to ZnAlg. Furthermore, the pyrolysis behavior was determined by pyrolysis–gas chromatography–mass spectrometry (Py-GC-MS) and the flame-retardant mechanism was proposed based on the combined experimental results. The prepared composites show promising application prospects in building materials and the textile industry.


2012 ◽  
Vol 466-467 ◽  
pp. 495-499 ◽  
Author(s):  
Ming Gao ◽  
Ying Juan Sun

A novel cheap macromolecular intumescent flame retardants (Zn-MIFR), was synthesized, and its structure was a caged bicyclic macromolecule containing phosphorus-silicon characterized by IR. Epoxy resins (EP) were modified with Zn-MIFR to get the flame retardant EP, whose flammability and burning behavior were characterized by UL 94, limiting oxygen index (LOI), dilatation, char yield, smoke density rating (SDR) and maximum smoke density (MSD). The epoxy resins were obtained for the UL 94 V-0 rating at low Zn contents of 3.0 % get a LOI of 27.5% and char yield of 20.5%. Dilatation, SDR and MSD of EP/Zn-MIFR decreased. The degradation behavior of the EP/Zn-MIFR was studied by TG and EDX analysis. The experimental results exhibited that the initial decomposition temperature (IDT) was decreased, integral procedure decomposition temperature (IPDT) and amounts of Zn and P at the residue were increased.


2012 ◽  
Vol 586 ◽  
pp. 172-176
Author(s):  
Hao Ran Zhou ◽  
Hao Cheng Yang ◽  
An Sun ◽  
Shuang Zhao

As the epoxy potting compound widely used, their flame retardant properties were concerned day by day.This paper neopentyl glycol phosphate melamine salt (NPM) was synthesised via phosphorus oxychloride as the acid source, neopentyl glycol as carbon source, melamine as gas source. The structure of NPM was characterized via infrared spectroscopic analysis (IR). Then the flame retardant properties of NPM/epoxy resin systerm were researched via the limiting oxygen index (LOI), vertical burning experiment, thermal gravimetric analysis (TGA) . The result shows that When the dosage of NPM is 27%, limiting oxygen index of epoxy resin have a extremum, is 32.4, char yield is 18.7% at 600°C. NPM can play a significant role in the improvement of the flame retardant properties of the epoxy.


2018 ◽  
Vol 42 (16) ◽  
pp. 13873-13883 ◽  
Author(s):  
Tianlu Xu ◽  
Chunling Zhang ◽  
Peihong Li ◽  
Xueyan Dai ◽  
Lijie Qu ◽  
...  

Polysiloxane foam (PSF) is a foam material with outstanding performance. However, the limiting oxygen index (LOI) of pure PSF is only 22.0 vol%, which can be attributed to combustible materials.


2021 ◽  
Author(s):  
Yajun Chen ◽  
Jingxiu He ◽  
Zhe Sun ◽  
Bo Xu ◽  
Juan Li ◽  
...  

Abstract Cellulose nanocrystals (CNCs) have been used as bio-based carbon source in intumescent system. However, CNCs have the disadvantages of low onset decomposition temperature and decompose and carbonize during processing. We, herein, demonstrated the design of phosphazene-containing CNCs (P/N-CNCs) with great thermal stability and outstanding charring ability. The TGA results showed that the initial decomposition temperature of P/N-CNCs was increased from 202.4 ℃ to 272.2 ℃ (increased by 34.5%), and the residual char at 700 ℃ was increased from 24.9 wt% to 55.8 wt% compared with CNCs. Then, flame retardant PLA composites were prepared by blending PLA, P/N-CNCs with ammonium polyphosphate (APP), melamine (MPP), aluminum hypophosphite (AHP) and piperazine pyrophosphate (PPAP), respectively. The thermal stability, flame retardant properties and mechanical properties of PLA composites were investigated. The results showed that the flame retardant system constructed by 7 wt% APP and 3 wt% P/N-CNCs had the best effect in PLA. PLA/7APP/3P/N-CNCs had the highest limit oxygen index value (28.1%), the lowest peak heat release rate (266 kW/m2) and reached UL 94 V-0 rating. Moreover, the tensile strength, impact strength and elongation at break of PLA/7APP/3P/N-CNCs were increased by 7.3%, 18.6% and 29.4%, respectively, compared with these properties of PLA/7APP/ 3CNCs. This work provides a new idea for the design of CNCs with great thermal stability and outstanding charring ability, and offers a new method for the preparation of high-performance flame-retardant PLA composites.


Polymers ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1562
Author(s):  
Yunxian Yang ◽  
De-Yi Wang ◽  
Laia Haurie ◽  
Zhiqi Liu ◽  
Lu Zhang

Some crop by-products are considered to be promising materials for the development of novel biobased products for industrial applications. The flammability of these alternatives to conventional materials is a constraint to expanded applications. Polylactide (PLA) composites containing a combination of oxidized corn pith fiber (OCC) and a biobased flame retardant (PA-THAM) have been prepared via an in situ modification method. SEM/EDS, FTIR and TGA were performed to establish that PA-THAM was coated onto the surface of OCC. The mechanical properties, thermal stability and fire behavior of PLA-based biocomposites were investigated. The incorporation of 5 phr PA-THAM imparted biocomposite good interfacial adhesion and increased decomposition temperature at 10% mass loss by 50 °C. The flame retardant properties were also improved, as reflected by an increased LOI value, a UL-94 V-2 rating, reduction of PHRR, and increased formation of char residue. Therefore, the introduction of 5 phr PA-THAM can maintain a good balance between flame retardancy and mechanical properties of this PLA/OCC system.


2019 ◽  
Vol 28 (3) ◽  
pp. 209-219 ◽  
Author(s):  
Na Wang ◽  
Lingtong Li ◽  
Yang Xu ◽  
Kun Zhang ◽  
Xiaolang Chen ◽  
...  

The flammability characterization and synergistic effects of red phosphorus masterbatch (RPM) with expandable graphite (EG) in flame-retardant polypropylene (PP)/thermoplastic polyurethane (TPU) composites are investigated by limiting oxygen index, UL-94 testing, cone calorimeter tests, thermal gravimetric analysis, Fourier transform infrared (FTIR), and scanning electron microscopy. The results show that the flame retardancy of PP/TPU/EG/RPM composites is greatly influenced by RPM. The synergistic effects between RPM and EG take place in the flame-retardant composites. The presence of RPM with EG decreases significantly the heat release rates and total heat release, and UL-94 V-0 rating is achieved when suitable amount of RPM substitutes for EG in the PP/TPU/EG/RPM composites. The T onset and T 10 wt% of the composites are improved because of the presence of RPM. The FTIR spectra show that the incorporation of RPM improves the thermo-oxidative stability of PP/TPU at higher temperatures. The morphological observations indicate the reinforcement of thermal stability, and flame-retardant performance is attributed to the compact and stable char layers promoted by RPM with EG acted as an effective heat barrier and thermal insulation.


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