Epoxy Resins Treated with Novel Silicon-Containing Flame Retardant

2012 ◽  
Vol 560-561 ◽  
pp. 563-568 ◽  
Author(s):  
Ming Gao ◽  
Ying Juan Sun

A novel cheap macromolecular intumescent flame retardants (Si-MIFR), was synthesized, and its structure was a caged bicyclic macromolecule containing phosphorus-silicon characterized by IR. Epoxy resins (EP) were modified with Si-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 Si contents of 3.0 % get a LOI of 27.5% and char yield of 23.8%. Dilatation, SDR and MSD of EP/Si-MIFR decreased. The degradation behavior of the EP/Si-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 Si and P at the residue were increased.

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.


2013 ◽  
Vol 648 ◽  
pp. 73-77
Author(s):  
Chun Feng Sun ◽  
Ming Gao

A novel cheap macromolecular intumescent flame retardants (Mg-MIFR), was synthesized, and its structure was a caged bicyclic macromolecule containing phosphorus- magnesium characterized by IR. Epoxy resins (EP) were modified with Mg-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 Mg contents of 4.0% get a LOI of 27.0% and char yield of 19.8%. Dilatation, SDR and MSD of EP/Mg-MIFR decreased. The degradation behavior of the EP/Mg-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 Mg and P at the residue were increased.


2014 ◽  
Vol 983 ◽  
pp. 171-174
Author(s):  
Fa Chao Wu ◽  
Shuang Tian ◽  
Song Liu

A novel cheap macromolecular intumescent flame retardants (Mn-MIFR), was synthesized. Epoxy resins (EP) were modified with Mn-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 Mn contents of 4.0 % get a LOI of 26.5% and char yield of 18.2%. Dilatation, SDR and MSD of EP/Mn-MIFR decreased. The degradation behavior of the EP/Mn-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 Mn and P at the residue were increased.


2013 ◽  
Vol 423-426 ◽  
pp. 574-577
Author(s):  
Yong Li Yang

A novel cheap macromolecular intumescent flame retardants (Al-MIFR), was synthesized, and its structure was a caged bicyclic macromolecule containing phosphorus-aluminum characterized by IR. Epoxy resins (EP) were modified with Al-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 Al contents of 4.0 % get a LOI of 26.8% and char yield of 19.5%. Dilatation, SDR and MSD of EP/Al-MIFR decreased. The degradation behavior of the EP/Al-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 Al and P at the residue were increased.


2013 ◽  
Vol 705 ◽  
pp. 101-105
Author(s):  
Qiu Ju Dai ◽  
Ming Gao

A novel cheap macromolecular intumescent flame retardants (Cu-MIFR), was synthesized, and its structure was a caged bicyclic macromolecule containing phosphorus-copper characterized by IR. Epoxy resins (EP) were modified with Cu-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 Cu contents of 3.0 % get a LOI of 27.0% and char yield of 19.4%. Dilatation, SDR and MSD of EP/Cu-MIFR decreased. The degradation behavior of the EP/Cu-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 Cu and P at the residue were increased.


2005 ◽  
Vol 13 (7) ◽  
pp. 697-707 ◽  
Author(s):  
Qiang Li ◽  
Pingkai Jiang ◽  
Zhanpai Su ◽  
Ping Wei

Flame retardants containing phosphorus, nitrogen and silicone elements have been synthesized. The thermal stabilities of polypropylene (PP), PSiN and PP/PSiN have been studied by thermogravimetric (TG) analysis in nitrogen, air and oxygen atmospheres. The initial decomposition temperature (IDT), maximum-rate degradation temperature (Tmax), integral procedure decomposition temperature (IPDT) and char yield at 800 °C in various atmospheres have been investigated. Although the IDT of PP was reduced by the introduction of PSiN, the Tmax, IPDT and char yield were all increased. The flame retardancy of PP/PSiN composites were evaluated by measuring their Limiting Oxygen Index (LOI) values. Their thermal stabilities agreed with the results of the flame retardancy tests: the PP/PSiN-A exhibited good flame retardancy with LOI of 26.0 and its char yields at 800 °C were 27 wt.% (in nitrogen), 12 wt.% (air) and 12 wt.% (in oxygen). The activation energies of PP, PSiN and PP/PSiN composites in various atmospheres were calculated using the method of Horowitz-Metzger.


Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2205
Author(s):  
Qian Li ◽  
Yujie Li ◽  
Yifan Chen ◽  
Qiang Wu ◽  
Siqun Wang

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.


2011 ◽  
Vol 197-198 ◽  
pp. 1346-1349 ◽  
Author(s):  
Fa Chao Wu

Bis(2,6,7-trioxa-l-phosphabicyclo[2.2.2]octane-4-methanol) melaminium salt (Melabis) and microcapsules of Melabis with melamine resin shell as flame retardants (FR), respectively, were synthesized. Their structures were characterized by NMR, IR, SEM, TG and element analysis. 20% weight of microcapsules was doped into epoxy resins (EP) to get 28.5 % of LOI and UL 94 V-0. The heat and smoke release of EP containing microcapsules was valued by cone calorimeter.


Polymers ◽  
2022 ◽  
Vol 14 (2) ◽  
pp. 245
Author(s):  
Yong Sun ◽  
Yongli Peng ◽  
Yajiao Zhang

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.


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.


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