Study on flame retardancy of TGDDM epoxy resin blended with inherent flame-retardant epoxy ether

2017 ◽  
Vol 30 (3) ◽  
pp. 318-327 ◽  
Author(s):  
Mengjiao Wang ◽  
Shijiang Fang ◽  
Heng Zhang
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Decomposition Temperature ◽  
Resin Matrix ◽  
Thermal Stabilities ◽  
Limiting Oxygen Index ◽  
Diaminodiphenyl Sulfone ◽  
Air Atmosphere ◽  
Index Value

In this article, inherent flame-retardant epoxy ether, 9,10-dihydro-9-oxa-10-[1,1-bis(4-glycidyloxyphenyl)ethyl]-10-phosphaphenanthrene 10-oxide (DPBAEP), with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide moieties was synthesized via an economical method and was used to improve the flame retardancy of 4,4′-tetradiglycidyl diaminodiphenyl methane (TGDDM). A series of epoxy resins were prepared and cured with 4,4′-diaminodiphenyl sulfone. The glass transition temperatures ( Tg) of resin composites were above 243°C and decreased only slightly after DPBAEP was added. The thermal stabilities under the nitrogen (N2) and air atmosphere were also measured using thermogravimetric analysis. The results indicated that DPBAEP had a high decomposition temperature and affected the thermal degradation and promoted the charring of resins. When only over 5 wt% of DPBAEP was introduced, the thermosets obtained a high limiting oxygen index value of around 33.0%, achieved vertical burning V-0 rating and presented fast-swelling char barriers. In order to better understand the flame-retardant mechanisms, the residual char was investigated by scanning electron microscopy observation and Fourier transform infrared spectra. We inferred that the phosphorus (P) moieties reacted with the resin matrix, which played a significant role in promoting the formation of char with special structure, as well as making it rich and tough enough. This kind of char barrier could protect the underlying resin matrix against oxygen and heat transfer and inhibited volatile combustible from diffusing to the flame. Hence, thanks to the synergistic effect of P–N and the excellent compatibility, DPBAEP could impart excellent flame retardancy to TGDDM epoxy resin.

Flammability and thermal properties of cotton fabrics modified with a novel flame retardant containing triazine and phosphorus components

2016 ◽  
Vol 87 (11) ◽  
pp. 1367-1376 ◽  
Author(s):  
Chaohong Dong ◽  
Zhou Lu ◽  
Peng Wang ◽  
Ping Zhu ◽  
Xuechao Li ◽  
...  
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Cotton Fabric ◽  
Flame Retardancy ◽  
Decomposition Temperature ◽  
Cotton Fabrics ◽  
Cone Calorimetry ◽  
Limiting Oxygen Index ◽  
Untreated Cotton ◽  
Index Value

A novel formaldehyde-free flame retardant containing phosphorus and dichlorotriazine components (CTAP) for cotton fabrics was synthesized. As an active group, the dichlorotriazine could react with cotton fabric via covalent reaction. The addition of 20.7 wt% CTAP into the cotton fabric obtained a high limiting oxygen index value of 31.5%, which was 13.5% higher than the pure cotton fabric. The results of heat release rate, total heat release and effective heat combustion indicated that CTAP effectively imparted flame retardancy to cotton fabric by the cone calorimetry test. With respect to the untreated cotton fabrics, the treated cotton fabrics degraded at lower decomposition temperature and form a consistent and compact char layer, which could be observed by thermogravimetric analysis, Fourier transform infrared spectroscopy and scanning electron microscopy. Compared to the untreated cotton fabrics, CTAP performed an effective role in flame retardancy for treated cotton fabrics. Meanwhile, it stimulated the formation of char and promoted the thermal stability of treated cotton fabrics during combustion.

A transparent and intumescent phosphaphenanthrene/phenylpyrazole-containing epoxy resin system and its flame retardancy

2021 ◽  
pp. 095400832199241
Author(s):  
Zijin Luo ◽  
Zhe Chen ◽  
Jun Wei ◽  
Dongchao Wang ◽  
Han Chen ◽  
...  
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Gas Chromatography Mass Spectrometry ◽  
Control Group ◽  
Pyrolysis Gas ◽  
Limiting Oxygen Index ◽  
Cone Calorimeter Test ◽  
Epoxy Resin System ◽  
Index Value

A novel intumescent flame retardant, PPMD, was designed from phosphaphenanthrene and nitrogen heterocycles through the two-step gut reactions of 1,4-phthalaldehyde and 3-methyl-1-phe-nylpyrazol-5-ylamine. After determination of its structure by nuclear magnetic resonance and Fourier-transform infrared analyses, PPMD was added to an epoxy resin (EP) to facilitate a curing process. Thus, EP/PPMD samples with excellent transparency and flame retardancy were acquired. For example, the EP sample satisfied the UL-94 V-0 standard and achieved a limiting oxygen index value of 30.5% because of the incorporation of 5 wt% PPMD. The cone calorimeter test of the EP/5% PPMD sample revealed that its total smoke production (TSP) and total heat release (THR) values of EP/5% PPMD was only 22.5% and 56.4% of the control group, respectively. Moreover, the average effective heat of combustion (av-EHC) value of EP/5% PPMD was reduced by 34.1%, indicating that PPMD possessed high flame-inhibition activity and smoke suppression efficiency. The flame-retardant mechanisms of PPMD were also investigated in gas phase by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and in condensed phase by XPS and IR.

scholarly journals An Effective Method for Preparation of Liquid Phosphoric Anhydride and Its Application in Flame Retardant Epoxy Resin

Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2205
Author(s):  
Qian Li ◽  
Yujie Li ◽  
Yifan Chen ◽  
Qiang Wu ◽  
Siqun Wang
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Epoxy Resins ◽  
Oxygen Index ◽  
Decomposition Temperature ◽  
Ease Of Use ◽  
Limiting Oxygen Index ◽  
Good Thermal Stability ◽  
Low Viscosity ◽  
The Impact

A novel liquid phosphorous-containing flame retardant anhydride (LPFA) with low viscosity was synthesized from 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and methyl tetrahydrophthalic anhydride (MeTHPA) and further cured with bisphenol-A epoxy resin E-51 for the preparation of the flame retardant epoxy resins. Both Fourier transform infrared spectroscopy (FT-IR), mass spectrometry (MS) and nuclear magnetic resonance (NMR) measurements revealed the successful incorporation of DOPO on the molecular chains of MeTHPA through chemical reaction. The oxygen index analysis showed that the LPFA-cured epoxy resin exhibited excellent flame retardant performance, and the corresponding limiting oxygen index (LOI) value could reach 31.2%. The UL-94V-0 rating was achieved for the flame retardant epoxy resin with the phosphorus content of 2.7%. With the addition of LPFA, the impact strength of the cured epoxy resins remained almost unchanged, but the flexural strength gradually increased. Meanwhile, all the epoxy resins showed good thermal stability. The glass transition temperature (Tg) and thermal decomposition temperature (Td) of epoxy resin cured by LPFA decreased slightly compared with that of MeTHPA-cured epoxy resin. Based on such excellent flame retardancy, low viscosity at room temperature and ease of use, LPFA showed potential as an appropriate curing agent in the field of electrical insulation materials.

scholarly journals A Study on the Synthesis, Curing Behavior and Flame Retardance of a Novel Flame Retardant Curing Agent for Epoxy Resin

Polymers ◽  
2022 ◽  
Vol 14 (2) ◽  
pp. 245
Author(s):  
Yong Sun ◽  
Yongli Peng ◽  
Yajiao Zhang
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Decomposition Temperature ◽  
Isothermal Kinetics ◽  
Flame Retardance ◽  
Curing Agent ◽  
Initial Decomposition Temperature ◽  
Limiting Oxygen Index ◽  
Epoxy Resin System ◽  
Dsc Method

In this work, a flame retardant curing agent (DOPO-MAC) composed of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide DOPO and methyl acrylamide (MAC) was synthesized successfully, and the structure of the compound was characterized by FT-IR and 1H-NMR. The non-isothermal kinetics of the epoxy resin/DOPO-MAC system with 1% phosphorus was studied by non-isothermal DSC method. The activation energy of the reaction (Ea), about 46 kJ/mol, was calculated by Kissinger and Ozawa method, indicating that the curing reaction was easy to carry out. The flame retardancy of the epoxy resin system was analyzed by vertical combustion test (UL94) and limiting oxygen index (LOI) test. The results showed that epoxy resin (EP) with 1% phosphorus successfully passed a UL-94 V-0 rating, and the LOI value increased along with the increasing of phosphorus content. It confirmed that DOPO-MAC possessed excellent flame retardance and higher curing reactivity. Moreover, the thermal stability of EP materials was also investigated by TGA. With the DOPO-MAC added, the residual mass of EP materials increased remarkably although the initial decomposition temperature decreased slightly.

scholarly journals Preparation and properties of flame-retardant epoxy resins containing reactive phosphorus flame retardant

2020 ◽  
Vol 15 ◽  
pp. 155892502090132
Author(s):  
Sang-Hoon Lee ◽  
Seung-Won Oh ◽  
Young-Hee Lee ◽  
Il-Jin Kim ◽  
Dong-Jin Lee ◽  
...  
Keyword(s):  
Impact Strength ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Epoxy Resins ◽  
Phosphorus Content ◽  
Phosphorus Compound ◽  
Phosphorus Compounds ◽  
Limiting Oxygen Index ◽  
The Impact

To prepare flame-retardant epoxy resin, phosphorus compound containing di-hydroxyl group (10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phospha phenanthrene-10-oxide, DOPO-HQ) was reacted with uncured epoxy resin (diglycidyl ether of bisphenol A, YD-128) and then cured using a curing agent (dicyandiamide, DICY). This study focused on the effect of phosphorus compound/phosphorus content on physical properties and flame retardancy of cured epoxy resin. The thermal decomposition temperature of the cured epoxy resins (samples: P0, P1.5, P2.0, and P2.5, the number represents the wt% of phosphorus) increased with increasing the content of phosphorus compound/phosphorus (0/0, 19.8/1.5, 27.8/2.0, and 36.8/2.5 wt%) based on epoxy resin. The impact strength of the cured epoxy resin increased significantly with increasing phosphorus compound content. As the phosphorus compound/phosphorus content increased from 0/0 to 36.8/2.5 wt%, the glass transition temperature (the peak temperature of loss modulus curve) increased from 135.2°C to 142.0°C. In addition, as the content of phosphorous compound increased, the storage modulus remained almost constant up to higher temperature. The limiting oxygen index value of cured epoxy resin increased from 21.1% to 30.0% with increasing phosphorus compound/phosphorus content from 0/0 to 36.8/2.5 wt%. The UL 94 V test result showed that no rating for phosphorus compounds less than 19.8 wt% and V-1 for 27.8 wt%. However, when the phosphorus compound was 36.8 wt%, the V-0 level indicating complete flame retardancy was obtained. In conclusion, the incorporation of phosphorus compounds into the epoxy chain resulted in improved properties such as impact strength and heat resistance, as well as a significant increase in flame retardancy.

scholarly journals Synergistic Flame Retardant Effect of Barium Phytate and Intumescent Flame Retardant for Epoxy Resin

Polymers ◽  
2021 ◽  
Vol 13 (17) ◽  
pp. 2900
Author(s):  
Linyuan Wang ◽  
Yue Wei ◽  
Hongbo Deng ◽  
Ruiqi Lyu ◽  
Jiajie Zhu ◽  
...  
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Barium Carbonate ◽  
Environmentally Friendly ◽  
Intumescent Flame Retardant ◽  
Limiting Oxygen Index ◽  
Application Range ◽  
Peak Heat Release Rate ◽  
Synergistic Flame Retardant

Recently, widespread concern has been aroused on environmentally friendly materials. In this article, barium phytate (Pa-Ba) was prepared by the reaction of phytic acid with barium carbonate in deionized water, which was used to blend with intumescent flame retardant (IFR) as a flame retardant and was added to epoxy resin (EP). Afterward, the chemical structure and thermal stability of Pa-Ba were characterized by Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA), respectively. On this basis, the flammability and flame retardancy of EP composites were researched. It is shown that EP/14IFR/2Ba composite has the highest limiting oxygen index (LOI) value of 30.7%. Moreover, the peak heat release rate (PHRR) of EP/14IFR/2Ba decreases by 69.13% compared with pure EP. SEM and Raman spectra reveal the carbonization quality of EP/14IFR/2Ba is better than that of other composites. The results prove that Pa-Ba can cooperate with IFR to improve the flame retardancy of EP, reducing the addition amount of IFR in EP, thus expanding the application range of EP. In conclusion, adding Pa-Ba to IFR is a more environmentally friendly and efficient method compared with others.

Synthesis of a Flame Retardant and Hydrophobic Epoxy Resin with Multiple Elements Synergistic Effect for Tunnel Seepage Prevention Application

2020 ◽  
Vol 842 ◽  
pp. 314-325
Author(s):  
Bin Lin
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Oxygen Index ◽  
Fire Retardant ◽  
Practical Application ◽  
Water Contact ◽  
Limiting Oxygen Index ◽  
New Perspective ◽  
Grouting Materials

Epoxy resin (EP) mortar usually used to repair the cracking of concrete structure under damp environment, but EP is extremely flammable, thus it’s extremely imperative to design a novel multifunction EP grouting materials with flame retardancy and waterproofness for the practical application. Targeting ingenious decoration of EP grouting materials, multiple flame retardant elements (phosphorus, nitrogen and fluorine) are concurrently introduced into a fire retardant and the fire retardant defined as DDM-FNP. The obtained DDM-FNP/EP grouting composite possess high thermal stability, flame retardancy and hydrophobicity. The limiting oxygen index (LOI) value of DDM-FNP/EP composites has a significant improve, which is increased from 26.7 (EP-0) to 35.8 (EP-4). Composites with more than 10 wt% of DDM-FNP could pass UL-94 V-0 rating without dripping. Compared with EP-0, the PHRR and THR of EP-4 are decreased by 31.1% and 21.6%, respectively. In addition, due to the introduction of the F element, the water contact angle of EP composites is changed from 75.2° (hydrophilicity) to 98.6° (hydrophobicity) after the introduction of a certain amount of DDM-FNP flame retardant. Therefore, this work provide a new perspective to design a multifunction EP grouting composite and improve the value of practical application on seepage prevention of tunnel.

scholarly journals PREPARATION OF IRON- REDUCED GRAPHENE OXIDE/ EPOXY RESIN COMPOSITE AND ITS FLAME RETARDANCY AND THERMAL STABILITY

10.6036/10327 ◽  
2022 ◽  
Vol 97 (1) ◽  
pp. 98-103
Author(s):  
XIAN WANG ◽  
JINLONG ZHUO ◽  
TIANQING XING ◽  
Xingran Wang
Keyword(s):  
Thermal Stability ◽  
Graphene Oxide ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Iron Powder ◽  
Flame Retardancy ◽  
Limiting Oxygen Index ◽  
Cone Calorimeter Test ◽  
Industrial Manufacture ◽  
Ul 94

In order to reduce flammability, smoke release and enhance thermal stability of epoxy resin (EP), iron powder is mixed with graphene oxide/ epoxy resin (GO/EP) composite by mechanical blending. The combustion performance of composite material is investigated through limiting oxygen index (LOI), Underwriters Laboratory (UL)-94 test, and cone calorimeter test (CCT). Thermogravimetric-Fourier transform infrared spectroscopy (TG-FTIR) and scanning electron microscope (SEM) are also used to explore the mechanism of flame retardancy and smoke suppression. Results show that, with the addition of 0.5% mass fraction of GO and the corresponding iron powder combination (EP3 sample), the LOI value can achieve 32.5% while reaching the UL-94 V0 rating. Compare with EP0, the peaks of heat release rate, smoke production rate, and smoke factor values of EP3 are decreased by 42%, 60%, and 50%, respectively. The char and TG-FTIR data of EP3 reveal that it has a more compact structure, good thermal stability, and produce fewer toxic gases and smoke. Reduction of GO could inhibit the degradation of EP, and iron catalyzes the formation of carbonaceous char on the surface. Thus, the thermal stability and flame retardancy of EP are improved significantly. This study provides a suitable way to prepare graphene/EP composites that contain iron catalyst and can be extended to the industrial manufacture of flame retardant polymer composites. Keywords: iron powder; epoxy resin; graphene oxide; flame retardant; thermal stability

Investigation of nickel ammonia phosphate with different morphologies as a new high-efficiency flame retardant for epoxy resin

2019 ◽  
Vol 32 (4) ◽  
pp. 359-370 ◽  
Author(s):  
Weiwei Zhang ◽  
Hongjuan Wu ◽  
Weihua Meng ◽  
Jiahe Li ◽  
Yumeng Cui ◽  
...  
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Photoelectron Spectroscopy ◽  
High Efficiency ◽  
Ammonium Phosphate ◽  
Cone Calorimetry ◽  
Limiting Oxygen Index ◽  
X Ray ◽  
The Matrix

Nanowires, nanosheets, and microflowers of nickel ammonium phosphate (NiNH4PO4·H2O) were synthesized by a mixed solvothermal method and used to improve the flame retardancy of epoxy resin (EP). The solvent concentration and surfactant content were found to play a key role in nucleation and growth of NiNH4PO4·H2O. The structure of NiNH4PO4·H2O was characterized by X-ray diffraction and X-ray photoelectron spectroscopy. The flame retardancy, thermostability, mechanical properties, and flame retardancy mechanism of EP/NiNH4PO4·H2O composites were analyzed using the limiting oxygen index (LOI), cone calorimetry (Cone), mechanical property tests, thermogravimetric analysis, and thermogravimetric–Fourier transform infrared spectroscopy. The results indicated that NiNH4PO4·H2O has proper thermal stability and greatly improves the flame retardancy of EP. The nanosheets outperformed the other morphologies; the EP/5% NiNH4PO4·H2O nanosheets have an LOI of 35.2%, which exceeds that of pure EP (24.7%). Furthermore, Cone showed that these nanosheets have the lowest peak heat release rate and peak smoke production rate, which are 69.1% and 36.5% lower than those of pure EP, respectively. NiNH4PO4·H2O can promote the formation of a stable char layer and release nonflammable gases, thus protecting the matrix by preventing heat and oxygen transfer and reducing the concentration of combustible gas. NiNH4PO4·H2O is expected to serve as a new high-efficiency flame retardant for EP.

Electrospun polyimide/organic montmorillonite composite nanofibrous membranes with enhanced mechanical properties and flame retardancy

2018 ◽  
Vol 49 (7) ◽  
pp. 875-888
Author(s):  
Liang Wang ◽  
Lingyan Cui ◽  
Jie Fan ◽  
Yong Liu
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Flame Retardancy ◽  
Decomposition Temperature ◽  
Limiting Oxygen Index ◽  
Organic Montmorillonite ◽  
Transmission Electron ◽  
Nanofibrous Membranes ◽  
Clay Layers ◽  
Index Value

Polyimide/organic montmorillonite nanofibrous membranes were fabricated through electrospinning of polyamic acid/organic montmorillonite precursors followed by a thermal imidization process. Scanning electron microscopy micrographs showed small amounts of organic montmorillonite addition (<3%) and increase in the diameter of polyimide nanofibers. However, higher organic montmorillonite fraction generated microspheres due to the aggregation of clay nanoplatelets. Transmission electron microscopy images indicated that both exfoliated and intercalated organic montmorillonites existed in polyimide nanofibers when low quantity of clay was loaded (<3%). As the clay amount increased, exfoliated structure disappeared and stacked clay layers were observed. The optimum concentration of organic montmorillonite is 3%. By incorporating 3% clay, the tensile strength and modulus of membrane increased by 92.1 and 48.6%, respectively. Moreover, the limiting oxygen index value arose from 29.2 to 30.4%. Higher thermal stability was also achieved because of the heat barrier effect of clay layers. The onset decomposition temperature increased by 17℃ by adding 5% clay. These results demonstrate that tiny organic montmorillonite incorporation is relatively effective for improving the mechanical properties as well as flame retardancy of polyimide nanofibrous membrane.

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