Synthesis and Structure of A Novel Caged Bicyclic Phosphate Flame Retardant

PI novel caged bicyclic phosphate flame retardant tri(1-oxo-2,6,7-trioxa-1-phosphabicyclo [2.2.2] octane-methyl) phosphate (Trimer) was synthesized from 1-oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo [2.2.2] octane (PEPA) and phosphorus oxychloride in this paper. Its structure was characterized by elemental analysis. FTIR, H-1 NMR. P-31 NMR and X-ray diffraction analysis.

FLAME RETARDANT OF GUANIDINE CONDENSED PHOSPHATE (GCP) FOR WOOD

GCP and APP were used as flame retardants for poplar wood and larch wood,and their flame retardancy(OI), permeability (Surface electron spectroscopy), water-re pellency and corrosion toward nail evaluated. The results showed that GCP is in advance of APP. From the thermal analysis and char composition analysis, it is concluded that GCP mainly functions in condensed phase.

Built-up Effect of Core Material for Microencapsulated Flame Retardant Containing Dimethyl Methyl Phosphate

The flame retardants containing organophosphorus compounds have extensively been used in the flame retarding of polymer materials. Among others, dimethyl methyl phosphate (DMMP) was applied in flame retarding of polyurethane owing to its so much merit. However, the water-soluble property of DMMP restricted its application in textile fabric. The flame retarding system containing DMMP will be microencapsulated to form a novel flame retardant that could be used in textiles. We have studied the built–up effect of DMMP with some inorganic compounds to improve the afterflame and afterglow suppression in the flame retarding system. The experimental data indicated that inorganic compounds containing various non-metal elements P, N, B and metal ions Mg2+, Al3+, Ca2+, Zn2+, Cu2+, Mn4+ could be applied in flame retarding systems as additives to effectively suppress afterflame or afterglow.

Thermal and Thermo-oxidative Degradation of Flame Retardant High Impact Polystyrene with Triphenyl Phosphate and Novolac Epoxy Resin

Thermal and thermo-oxidative decomposition and decomposition kinetics of flame retardant high impact polystyrene （HIPS） with triphenyl phosphate （TPP） and novolac type epoxy resin （NE） were characterized using thermo-gravimetric experiment. And the flammability was determined by limited oxygen indices （LOI）. The LOI results show that TPP and NE had a good synthetic effect on the flame retardancy of HIPS. Compared with pure HIPS, the LOI values of HIPS/NE and HIPS/TPP only increased by about 5%, and the LOI value of HIPS/TPP/NE reached 42.3%, nearly 23% above that of HIPS. All materials showed one main decomposition step, as radical HIPS scission predominated during anaerobic decomposition. TPP increased the activity energy effectively while NE affected the thermal-oxidative degradation more with the help of the char formation. With both TPP and NE, the materials could have a comparable good result of both thermal and thermal-oxidative degradation, which could contribute to their effect on the flame retardancy.

Effect of Styrene on the Properties of Transparent Flame Retardant Unsaturated Phosphate Copolymer

The effect of styrene on unsaturated phosphate ester polymers was investigated. Copolymerization was carried out by adding different proportions of styrene when the unsaturated phosphate was polymerized to obtain an unsaturated phosphate-styrene copolymer. The structure and crosslink density of the copolymer was determined by fourier transform infrared (FTIR) spectra and gel fraction (G) testing. The heat resistance and flame retardancy of the polymer were tested by thermogravimetric (TGA) analysis, limiting oxygen index (LOI) and micro-combustion calorimeter (MCC). The infrared test proved that the styrene was successfully introduced into the polymer system. The gelation test results showed that the introduction of the rigid benzene ring increased the crosslink density of the copolymer. The tensile strength increased from 17.84 MPa to 34.63 MPa, and the impact strength remained stable within a certain range. At the same time, the solid ultraviolet absorption test results showed that the light transmittance of the materials was higher than 90%. The TG and DTG spectra showed that the heat resistance of the polymer was improved, but the residual carbon ratio was reduced from 30.47% to 25.54%. The LOI value decreased from 29.0% to 26.1%, and the UL-94 vertical burn rating was all V-0.

Biobased Furfurylated Poplar Wood for Flame-Retardant Modification with Boric Acid and Ammonium Dihydrogen Phosphate

Furfurylated wood exhibits excellent dimensional stability and corrosion resistance,making it a promising material for constructing buildings,but it is highly flammable.Herein,flame-retardant furfurylated poplar wood was produced via a two-step process utilizing boric acid(BA)and ammonium dihydrogen phosphate(ADP)as flame-retardant components,and biomass-derived furfuryl alcohol(FA)as a modifier.The acidity of BA and ADP allowed them to catalyze the polymerization of FA,which formed a cross-linked network that immobilized BA and ADP inside the wood.The addition of BA/ADP substantially delayed the time to ignition from 10 to 385 s and reduced the total heat release and total smoke release by 58.75%and 77.31%,respectively.Analysis of the pyrolysis process showed that the decomposition products of BA and ADP protected the underlying furfurylated wood and diluted combustible gases.This method significantly improved the fire retardancy and smokeless properties of furfurylated wood,providing promising prospects for its application as an engineering material.

Preparation of Polyurea Elastomer with Flame Retardant, Insulation and Thermal Conductivity Properties

By using 6,6-((sulfonylbis(4,1-phenylene)bis(azanediyl))bis(thiophen-2-ylm-ethylene))bis6H-di-benzo[c,e][1,2]oxaphosphinine 6-oxide(DOPO-N)as phosphorus-nitrogen flame retardant,the polyurea(PUA)with flame retardant properties(PUA/DOPO-N)was prepared.In addition,organically modified montmorillonite(OMMT)and magnesium hydroxide(MH)were used as co-effectors respectively,and the flame retardant PUA(PUA/DOPO-N/OMMT and PUA/DOPO-N/MH)were also prepared.Thermal properties,flame retardant properties,flame retardant mechanism and mechanical properties of PUA/DOPO-N,PUA/DOPO-N/OMMT and PUA/DOPO-N/MH were investigated by thermogravimetric(TG)analysis,limiting oxygen index(LOI),UL 94,cone calorimeter test,scanning electron microscopy(SEM),and tensile test.The results show that the LOI value of PUA/20%DOPO-N,PUA/18%DOPO-N/2%OMMT and PUA/15%DOPO-N/5%MH are 27.1%,27.7%,and 28.3%,respectively,and UL 94 V-0 rating is attained.Compared with PUA,the peak heat release rate(pk-HRR),total heat release(THR)and average effective heat combustion(av-EHC)of PUA/20%DOPO-N,PUA/18%DOPO-N/2%OMMT and PUA/15%DOPO-N/5%MH decrease significantly.SEM results indicate that the residual chars of PUA/20%DOPO-N,PUA/18%DOPO-N/2%OMMT and PUA/15%DOPO-N/5%MH are completer and more compact.The complex of DOPO-N/OMMT and DOPO-N/MH have synergistic flame retardancy.The mechanical properties of PUA can be improved by the addition of DOPO-N,DOPO-N/OMMT and DOPO-N/MH,respectively.The insulation performance test shows that the volume resistivity of PUA/20%DOPO-N is 6.25×10^(16)Ω.cm.Furthermore,by using modified boron nitride(MBN)as heat dissipating material,the complex of PUA/MBN was prepared,and the thermal conductivity of PUA/MBN was investigated.The thermal conductivity of PUA/8%MBN complex coating at room temperature is 0.166 W/(M·K),which is a 163%improvement over pure PUA.

Research Progress in Flame Retardant in Flame Retardant Coatings

Flame retardant coatings are functional materials that can serve as decorative and protec-tive substrates in the event of a fire.Flame retardant coatings generally consist of two parts:a base material and a flame retardant agent.A detailed introduction was given to the development of flame retardant coatings in recent years and the flame retardants used in flame retardant coatings.Flame retardants mainly include halogen flame retar-dants,phosphorus nitrogen flame retardants,expansion flame retardants,biomass flame retardants,and graphene flame retardants.The application of flame retardant coatings in the fields of epoxy resin,polyurethane,etc.was elaborated.In addition,the application of new biomass flame retardants and graphene flame retardants was introduced,and the future development of flame retardant coatings and flame retardants was described.

Microencapsulated ammonium polyphosphate by polyurethane with segment of dipentaerythritol and its application in flame retardant polypropylene

Dipentaerythritol(DPER),4,40-diphenylmethanediisocyanate(MDI)and melamine(MEL)are used as raw materials to microencapsulate ammonium polyphosphate(MAPP)in situ polymerization.The MAPP is characterized by Fourier transform infrared(FT-IR),scanning electron microscopy(SEM),transmission electron microscopy(TEM)and thermal gravimetric analysis(TGA).The results show that the coating operation can effectively improve water resistance of ammonium polyphosphate(APP),and MAPP has higher residual rate than that of APP after combustion.The flame retardant action of MAPP and APP in polypropylene(PP)is investigated by the limited oxygen index(LOI),vertical burning test(UL-94),TGA,SEM,and cone calorimeter test(CCT).The LOI value of the PP/MAPP composite at the same loading is higher than that of PP/APP composite.UL 94 ratings of PP/MAPP composites are raised to V-0 at 20 wt%loading.The results of CCT also show that MAPP is more efficient than APP.The morphological structures observed by digital photos and SEM demonstrated that MAPP could be promoted to form the continuous and compact intumescent char layer.The flame retardant mechanism of PP/MAPP is also discussed.

Synergistic Flame Retardant Effect of Ammonium Polyphosphate and Aluminum Hydroxide on Polyurethane

The flame-retardant properties of polyurethane(PU)containing ammonium polyphosphate(APP)and aluminum hydroxide(ATH)were investigated.Moreover,the flame retardant performance was investigated through thermogravimetric analysis,limiting oxygen index(LOI),vertical combustion(UL 94),and cone calorimeter.When 15 wt%APP and 5 wt%ATH were added together,the PU/15%APP/5%ATH sample shows better thermal stability and flame-retardant properties.When 15 wt%APP and 5 wt%ATH were added together,the LOI value of the PU/15%APP/5%ATH sample was 30.5%,and UL 94 V-0 rating was attained.Compared with PU,the peak heat release rate(PHRR),total heat release(THR),and average effective heat combustion(av-EHC)of the PU/15%APP/5%ATH sample decreased by 43.1%,21.0%,and 29.4%,respectively.In addition,the flame-retardant mechanism was investigated through cone calorimeter.The APP/ATH addition simultaneously exerted condensed phase and gas phase flame retardant effects.APP and ATH have synergistic flame retardant properties.

Synthesis of Organic-Inorganic Hybrid Aluminum Hypophosphite Microspheres Flame Retardant and Its Flame Retardant Research on Thermoplastic Polyurethane

Aluminum hypophosphite microspheres(AHP) were synthesized by hydrothermal method using NaH2PO2·H2O and AlCl3·6H2O as raw materials, and then the AHP microspheres were polymerized by surface polymerization of micro-nanospheres with cyclic cross-linked poly(cyclotriphosphazene-co-4,4'-sulfonyldiphenol)(PZS). A new organic-inorganic poly(phosphonitrile)-modified aluminum hypophosphite microspheres(PZS-AHP) were synthesized by encapsulation and applied to flame retardant thermoplastic polyurethane(TPU). The microstructure and chemical composition of the PZS-AHP microsphere were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray spectroscopy. The thermal stability of PZS-AHP microsphere was explored with thermogravimetric analysis. Thermogravimetric data indicate that the PZS-AHP microspheres have excellent thermal stability. The thermal and flame-retarding properties of the TPU composites were evaluated by thermogravimetric(TG), limited oxygen index tests(LOI), and cone calorimeter test(CCT). The TPU composite achieved vertical burning(UL-94) V-0 grade and LOI value reached 29.2% when 10 wt% PZS-AHP was incorporated. Compared with those of pure TPU, the peak heat release rate(pHRR) and total heat release(THR) of TPU/10%PZS-AHP decreased by 82.2% and 42.5%, respectively. The results of CCT indicated that PZS-AHP microsphere could improve the flame retardancy of TPU composites.

Increasing the Burned Time and Mechanical Properties with New Mix As Flame Retardant Based in Hexametaphosphate of Sodium and Borax in Textile 100% Acrylic Fabrics

It has been worked with textile fabrics of Acrylic 100 % , that have as final use the Tapestry, this fabrics have been impregnated with a two products flame retardant: Commercial Retardant, which is formed by a combination of a resin polymeric and acid phosphoric and Borax (Na2B4O5(OH)4.8H2O) with Sodium Hexametaphosphate (Na16P14O43). These Retardants?? has the advantage of the fact that it can be applied to the substrates mixed with water in the relation 1:1, 1:2 or pure. In order to reduce the flammability, Textile fabrics are coated with flame retardants. The flame retardant capabilities, mechanical properties and structural characteristics of the textile fabrics before and after the use of these products were investigated throughout the special textile methods for inflammability and mechanical resistibility. After the use of the flame retardants the mechanical properties of the fabrics were improved or at least remained the same as compared to fabrics without any treatment. The use of Borax / Sodium Hexametaphosphate /Water results in the essential increase of combustion retardation time about 2 minutes as compared with 8 seconds for untreated fabrics.

Research on the effect of the common flame retardant in reducing the flammability of the bitumen

The bituminous defect that the binder is flammable will bring road safety risk.Once it catches fires,large quantities of heat,smoke and poisonous gas are produced,released and spread quickly,which seriously hinder escape and rescue and harms heavily traffic safety.The common flame retardant system is used to modify the asphalt.Cone Calorimeter is adopted to evaluate the burning property of asphalt.The performance of the flame retardant is evaluated by limiting oxygen index and orthogonal design method.The paper analyzes the synergism of the asphalt and flame-retardant,and analyzes the effect of the flame on preventing the smoke to spread and demonstrates that the use of common flame retardants which is added into binder is good at reducing the flammability of the binder.This way can increase the safety of asphalt pavement when fire occurs in the tunnel.The study suggests that flame retardancy of asphalt can be evaluated by Limit Oxygen Index (LOI) and the flame retardancy property of asphalt has marked change according to the content of flame retardant.SB has perfect flame retardancy property,and ATH is better than MH in the effect of flame retardant.

Levels and distribution of brominated flame retardants in the soil of Harbin in China

This study reports the presence of brominated flame retardants in the topsoil in and around Harbin, a city in northeastern China. Samples of soil were collected from 17 locations in 2006, and the levels of 9 polybrominated diphenylethers （PBDEs 17, 28, 47, 66, 99, 100, 153, 154, and 183） ranged from 2.45 to 55.9 pg/g dry weight （dw） with a mean of 26.3 pg/g dw. These levels are very low comparing with those for some cities in Europe and USA. BDE 209 and hexabromocyclododecane were the two dominant congeners, with mean concentrations of 520 pg/g dw and 1750 pg/g dw, respectively. The concentrations of the total nine PBDE congeners clearly decreased from urban areas to background, but the compositions of individual congeners differed. Proportions of heavier congeners decreased while those of lighter congeners increased, along urban-rural-background transect, providing evidence for an urban fractionation effect. Correlation analysis indicated similar sources for PBDEs, hexabromocyclododecane, and 1,2-bis（2,4,6-tribromophenoxy）-ethane from urban areas but pentabromoethylbenzene was probably present due to long-range atmospheric transport. Principal component analysis was used to determine the characteristics of the relationships among these brominated flame retardants in the field.

Synthesis and Application of Novel Triazine-Based Charring-Foaming Agents in Intumescent Flame Retardant Polypropylene

Three novel triazine-based charring-foaming agents (M2-CFA, M4-CFA, and M6-CFA) were synthesized successfully with only water as the solvent and were characterized by FT-IR and thermal gravimetric analysis (TGA). These three charring-foaming agents and the byproduct 944-by were employed to study the effectiveness of the novel intumescent flame retardant dopant on the fire retardancy of polypropylene(PP) investigated through UL-94 and limiting oxygen index (LOI) tests. TGA results showed that the M4-CFA presented good char formation ability (char residue: 26.8% at 700 °C). It was found that the sample with a 2/1 mass ratio of APP to M4-CFA exhibited the best flame retardancy among all the PP composites: 35.5% LOI and a V-0 rating of UL-94. Additionally, the microstructure and morphology of char residues were further studied by XRD, Raman spectroscopy and SEM. © 2017, Tianjin University and Springer-Verlag Berlin Heidelberg.

Synthesis and thermal stability of a novel phosphorus-nitrogen containing intumescent flame retardant

A novel phosphorus-nitrogen containing intumescent flame retardant （P-N IFR） was prepared via the reaction of dichlor-opentate with N-methylaniline. The structure of the product was confirmed by ^1H NMR, ^31p NMR, MS and IR. TGA analysis showed it has effective thermal stability.

A NEW SYNERGIST FOR INTUMESCENT FLAME RETARDANT POLYPROPYLENE

The synergistic effects of silicotungstic acid (SiW12) as a catalyst in the phosphorus-nitrogen compounds AM-based intumescent flame-retardant (IFR) polypropylene (PP) were studied using the limiting oxygen index (LOI), the UL-94 test, thermogravimetric analysis (TGA), real time Fourier transform infrared (FTIR), laser Raman spectroscopy (LRS). The LOI data show that SiW12 added to PP/IFR systems has a synergistic FR effect with an IFR additive named AM. The TGA data show that SiW12 apparently increases the thermal stability of the PP/IFR systems at high temperature (T > 500degreesC). The FTIR results provide the positive evidence that IFR can improve the thermal stability of PP and SiW12 can induce a higher rate of formation of phosphoric acid and its derivatives. The LRS measurements provide useful information on the carbonaceous microstructures. In short, a suitable amount of SiW12 (1.5 wt%) exerts synergistic effects with the IFR by increasing the LOI value and the thermal stability at high temperature and promoting the formation of charred structures on the burning PP surface.

Effect of Flame Retardant Containing Phosphorus and Silicone on Thermal Performance of PC/ABS

A flame retardant （DPA-SiN） containing phosphorus, nitrogen and silicon elements was synthesized. The halogen free flame retardant was incorporated into PC/ABS to improve its flame retardancy. The flame-retardant properties of the PC/ABS/DPA-SiN blends were estimated by limiting oxygen index （LOI） values and CONE Calorimeter, while thermal stabilities were investi- gated through thermo gvavimetric analysis （TGA）. The PC/ABS/DPA-SiN blends were thermally degraded at 400℃ for different amounts of time and studied by Fourier transform infrared spectroscopy （FTIR） to better understand the degradation behavior of PC/ABS/DPA-SiN.

Synergistic effect of MXene on the flame retardancy and thermal degradation of intumescent flame retardant biodegradable poly(lactic acid)composites

The effect of Ti3C2 MXene nanosheets on the intumescent flame retardant(IFR)poly(lactic acid)(PLA)composites was investigated among a series of PLA/IFR/MXene,which were prepared by melt blending 0-2.0 wt%MXene,10.0 wt%-12.0 wt%IFR and PLA together.The results of limiting oxygen index(LOI)and vertical burning(UL-94)discover that the combination of 0.5 wt%MXene and 11.5 wt%IFR synergistically improves the fire safety of PLA to reach UL-94 V-0 rating with LOI value of 33.0%.The PLA/IFR/MXene composites perform an obvious reduction in peak of heat release rate(HRR)in cone calorimeter tests(CCTs).Furthermore,the carbon residues after CCTs were characterized by scanning electron microscope(SEM),laser Raman spectroscopy(LRS),X-ray diffraction(XRD)and X-ray photoelectron spectroscopy(XPS).It is demonstrated that both the titanium composition of the MXene structure and the characteristics of the two-dimensional material enhance the PLA/IFR/MXene composite materials’ability to produce a dense barrier layer to resist burnout during thermal degradation.

Hyperbranched Polyurethane Acrylate Applied to UV Curable Flame Retardant Coatings

UV curable hyperbranched prepolymers based on amine-ester, ester-amide and ether-amide started with AB_2-type monomers have been prepared by the authors. A series of work on allyl ether maleate hyperbranched polyesters for UV curing coatings by Hult and his colleagues has been reported. However, the UV cured films from those materials are all flammable when attached to fire without addition of flame retardants.