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, M...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.展开更多
A novel halogen-free phosphorus–nitrogen–silicon flame retardant monomer with reactive siloxy groups,N-(diphenylphosphino)-1,1-diphenyl-N-(3-(triethoxysilyl)propyl) phosphinamine(DPTA) has been synthesized and was a...A novel halogen-free phosphorus–nitrogen–silicon flame retardant monomer with reactive siloxy groups,N-(diphenylphosphino)-1,1-diphenyl-N-(3-(triethoxysilyl)propyl) phosphinamine(DPTA) has been synthesized and was applied to the fire-resistant finishing of cotton fabrics. The molecular structure of DPTA has been well characterized by elemental analysis, FTIR,1H NMR, and ^(31)P NMR spectroscopies. The chemically-grafted cotton fabrics, which were treated with 25 wt% DPTA, were obtained and confirmed by attenuated total reflectance Fourier infrared spectroscopy(ATR-FTIR). The flame retardancy and thermal property of the treated samples were investigated by limited oxygen index(LOI), vertical flammability test(VFT), thermogravimetric analysis(TGA) and microscale combustion calorimeter(MCC). It is noted that in vertical flammability test, the treated samples extinguished immediately upon removing the ignition source, whereas the untreated one was completely burned out. Furthermore, TGA and MCC tests revealed that the treated samples produced a high char formation and a low heated release during combustion. The surface morphology of the untreated and treated samples and the char residues after LOI tests were observed by scanning electron microscopy(SEM). Therefore, all the results showed that the treated cotton fabrics with 25 wt% DPTA apparently improved the fireresistant and thermal performances.展开更多
The effects of a magnesium-based layered composite on the flammability of a phenolic epoxy resin(EP)are studied.In order to produce the required composite material,first,magnesium hydroxide,aluminum salt and deionized...The effects of a magnesium-based layered composite on the flammability of a phenolic epoxy resin(EP)are studied.In order to produce the required composite material,first,magnesium hydroxide,aluminum salt and deionized water are mixed into a reactor according to a certain proportion to induce a hydrothermal reaction;then,the feed liquid is filtered out using a solid-liquid separation procedure;finally,the material is dried and crushed.In order to evaluate its effects on the flammability of the EP,first,m-phenylenediamine is added to EP and vacuum defoamation is performed;then,EP is poured into a polytetrafluoroethylene mold,cooled to room temperature and demoulded;finally,the magnesium-based layered composite is added to EP,and its flame retardance is characterized by thermogravimetric analysis,limiting oxygen index and cone calorimetry.The X-ray diffraction patterns show that the baseline of magnesium-based layered composite is stable and the front shape is sharp and symmetrical when the molar ratio of magnesium to aluminium is 3.2:1;with the addition of magnesium-based layered composite,the initial pyrolysis temperature of EP of 10%,15%and 30%magnesium-based layered composite decreases to 318.2°C,317.9°C and 357.1°C,respectively.After the reaction,the amount of residual carbon increases to 0.1%,3.45%and 8.3%,and the limiting oxygen index increases by 28.3%,29.1%and 29.6%,respectively.The maximum heat release rate of cone calorimeter decreases gradually.The optimum molar ratio of Mg:Al for green synthesis is 3.2:1,and the NO_(3)-intercalated magnesium-based layered composite has the best flame retardance properties.展开更多
Aluminum-oxide-hydroxide （AIOOH） is a clean and non-toxic flame retardant. There have been many trials for the fabrication of ultrafine AIOOH, Two main approaches exist for nano-AlOOH synthesis： reactive precipitat...Aluminum-oxide-hydroxide （AIOOH） is a clean and non-toxic flame retardant. There have been many trials for the fabrication of ultrafine AIOOH, Two main approaches exist for nano-AlOOH synthesis： reactive precipitation and batch hydrothermal synthesis, Both approaches are laborious and time consuming with poor control of particle morphology. We report on the novel continuous flow manufacture of AIOOH nanorods with controlled morphology （particle size and shape） by hydrothermal synthesis. AIOOH was harvested from its mother liquor （colloidal solution） using poly（acrylamide-co-acrylic acid） copolymer as a flocculating agent. The developed AIOOH shape and size, crystalline phase, thermal stability, and endothermic heat sink action were investigated by transmission electron microscopy, X-ray diffractome- try, thermogravimetric analysis, and differential scanning calorimetry, respectively. The phase transition of AlOOH to Al2O3 was demonstrated by conducting different X-ray diffractometry scans from 400 to 700℃. These results may provide an option for the continuous synthesis of nano-AIOOH as a clean and non-toxic flame retardant with excellent thermal stability. Consequently, enhanced flammability properties can be achieved at low solids loading.展开更多
Nanoparticles can provide flame retardance to hosting polymers and act as nano fire extinguishers. Hydroxyapatite （Ca5（OH）（PO4）3） （HA） is not hygroscopic, and is thermally stable up to 800℃, with 18.5 wt% pho...Nanoparticles can provide flame retardance to hosting polymers and act as nano fire extinguishers. Hydroxyapatite （Ca5（OH）（PO4）3） （HA） is not hygroscopic, and is thermally stable up to 800℃, with 18.5 wt% phosphorous content. It is this high phosphorous content that can provide HA with flame retardant properties. In this paper, we report on the continuous synthesis of ultrafine HA using a hydrothermal synthesis technique. The HA surface properties were changed from hydrophilic to hydrophobic by post-synthesis surface modification. The ratio of the HA nanoparticles and an intumescent agent known as Exolit AP750 was investigated to yield a self-extinguishing multi-component epoxy nanocomposite for extended application under extreme fire conditions. The HA/AP750/epoxy nanocomposite was able to resist a flame at 1700 oc and self-extinguish after the flame had been removed. The nanocomposite showed an enhanced flammability performance in standard cone calorimetry testing and formed a compact and cohesive protective char layer with a 50% decrease in peak heat released compared with virgin epoxy. Our aim was to establish the use of HA as an effective nanofiller with phosphorous-based flame retardant properties. The surface of this nano fire extinguisher was modified effectively with different surfactants for enhanced compatibility with different polymeric matrices.展开更多
Red phosphorus （RP） has attracted considerable attention as the anode for high-performance Na-ion batteries, owing to its low cost and high theoretical specific capacity of -2,600 mAh/g. In this study, a facile sing...Red phosphorus （RP） has attracted considerable attention as the anode for high-performance Na-ion batteries, owing to its low cost and high theoretical specific capacity of -2,600 mAh/g. In this study, a facile single-step flash-heat treatment was developed to achieve the reduction of graphene oxide （GO） and the simultaneous deposition of RP onto the reduced graphene oxide （rGO） sheets. The resulting RP/rGO composite was shown to be a promising candidate for overcoming the issues associated with the poor electronic conductivity and large volume variation of RP during cycling. The RP/rGO flexible film anode delivered an average capacity of 1,625 mAh/g during 200 cycles at a charge/ discharge current density of 1 A/g. Average charge capacities of 1,786, 1,597, 1,324, and 679 mAh/g at 1, 2, 4, and 6 A/g current densities were obtained in the rate capability tests. Moreover, owing to the RP component, the RP/rGO film presented superior flame retardancy compared to an rGO film. This work thus introduces a highly accessible synthesis method to prepare flexible and safe RP anodes with superior electrochemical performance toward Na-ion storage.展开更多
A phosphorus-nitrogen containing flame retardant additive of poly（phosphoric acid piperazine）, defined as PPAP, was synthesized by the salt-forming reaction between anhydrous piperazine and phosphoric acid, and the ...A phosphorus-nitrogen containing flame retardant additive of poly（phosphoric acid piperazine）, defined as PPAP, was synthesized by the salt-forming reaction between anhydrous piperazine and phosphoric acid, and the dehydration polymerization under heating in nitrogen atmosphere. Its chemical structure was well characterized by Fourier transform infrared（FTIR） spectroscopy, ^（13）C and ^（31）P solid-state nuclear magnetic resonance measurements. The synthesized PPAP and curing agent m-phenylenediamine were blended into epoxy resin（EP） to prepare flame retardant EP thermosets. The effects of PPAP on the fire retardancy and thermal degradation behavior of cured EP/PPAP composites were investigated by limiting oxygen index（LOI）, vertical burning（UL-94）, thermogravimetric analysis/infrared spectrometry（TG-IR） and cone calorimeter tests. The morphologies and chemical compositions of char residues for cured epoxy resin were investigated by scanning electron microscopy（SEM） and X-ray photoelectron spectroscopy（XPS）, respectively. The results demonstrated that the flame retardant EP thermosets successfully passed UL-94 V-0 flammability rating and the LOI value was as high as 30.8% when incorporating 5 wt% PPAP into the EP thermosets. The TGA results indicated that the synthesized PPAP flame retardant additive possessed high thermal stability and excellent charring capability. Meanwhile, the incorporation of PPAP stimulated the epoxy resin matrix to decompose and charring ahead of time due to its catalytic decomposition effect, which led to a higher char yield at high temperature. The morphological structures and the analysis results of XPS for char residues of EP thermosets revealed that the introduction of PPAP benefited the formation of a sufficient, more compact and homogeneous char layer containing phosphorus-nitrogen flame retardant elements on the material surface during combustion. The formed char layer with high quality effectively prevented the heat transmission and diffusion, limited the production of combustible gases, and inhibited the emission of smoke, leading to the reduction of heat and smoke release.展开更多
Eight dialkyl tetrabromophthalates (DATBPs) were synthesized by reacting tetrabromophthalic anhydride with excess alcohols which were used not only as a reactant but also as a solvent and using a quaternary ammonium s...Eight dialkyl tetrabromophthalates (DATBPs) were synthesized by reacting tetrabromophthalic anhydride with excess alcohols which were used not only as a reactant but also as a solvent and using a quaternary ammonium salt as a phase transfer catalyst (PTC). The yields were found to be between 85-93%. Their structures were characterized by IR, NMR and elementary analysis. The flame retardant properties of the compounds were also studied.展开更多
Some organoboron compounds as flame-retardants for fiber materials were prepared.Flame-retarding properties of these compounds determined by the Oxygen-Index Method weregood.These new compounds were characterized by I...Some organoboron compounds as flame-retardants for fiber materials were prepared.Flame-retarding properties of these compounds determined by the Oxygen-Index Method weregood.These new compounds were characterized by IR,~1H NMR spectrum and elementalanalysis.展开更多
The synthesis, properties and flame retardation of two kinds of flame retardants, mono(1 chloride 2 hydroxy propyl) phosphate and antimony mono(1 chloride 2 hydroxy propyl)phosphate were reported. Mono(1 chloride 2 hy...The synthesis, properties and flame retardation of two kinds of flame retardants, mono(1 chloride 2 hydroxy propyl) phosphate and antimony mono(1 chloride 2 hydroxy propyl)phosphate were reported. Mono(1 chloride 2 hydroxy propyl) phosphate was synthesized from epichlorohydrin and phosphoric acid at molar ratio of 1∶1.2 in the solvent of methyl benzene with AlCl 3 catalyst under the conditions of reaction temperature of 90 ℃ and reaction time of 2 h, its total yield is 82.5%. Antimony mono(1 chloride 2 hydroxy propyl)phosphate was synthesized from mono(1 chloride 2 hydroxy propyl)phosphate and antimony trioxide in the solvent of dimethyl sulfoxide with oxalic acid catalyst under the conditions of reaction temperature of 92 ℃ and reaction time of 4 h, the total yield is 85.6%. The physical chemical properties of the products were determined. When adding 15% of mono(1 chloride 2 hydroxy propyl) phosphate and antimony mono(1 chloride 2 hydroxy propyl)phosphate in polyethylene respectively, the oxygen indexes (OI) are 31.4 and 33.7 respectively. [展开更多
文摘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.
基金Supported by the National Natural Science Foundation of China(21301160)
文摘A novel halogen-free phosphorus–nitrogen–silicon flame retardant monomer with reactive siloxy groups,N-(diphenylphosphino)-1,1-diphenyl-N-(3-(triethoxysilyl)propyl) phosphinamine(DPTA) has been synthesized and was applied to the fire-resistant finishing of cotton fabrics. The molecular structure of DPTA has been well characterized by elemental analysis, FTIR,1H NMR, and ^(31)P NMR spectroscopies. The chemically-grafted cotton fabrics, which were treated with 25 wt% DPTA, were obtained and confirmed by attenuated total reflectance Fourier infrared spectroscopy(ATR-FTIR). The flame retardancy and thermal property of the treated samples were investigated by limited oxygen index(LOI), vertical flammability test(VFT), thermogravimetric analysis(TGA) and microscale combustion calorimeter(MCC). It is noted that in vertical flammability test, the treated samples extinguished immediately upon removing the ignition source, whereas the untreated one was completely burned out. Furthermore, TGA and MCC tests revealed that the treated samples produced a high char formation and a low heated release during combustion. The surface morphology of the untreated and treated samples and the char residues after LOI tests were observed by scanning electron microscopy(SEM). Therefore, all the results showed that the treated cotton fabrics with 25 wt% DPTA apparently improved the fireresistant and thermal performances.
文摘The effects of a magnesium-based layered composite on the flammability of a phenolic epoxy resin(EP)are studied.In order to produce the required composite material,first,magnesium hydroxide,aluminum salt and deionized water are mixed into a reactor according to a certain proportion to induce a hydrothermal reaction;then,the feed liquid is filtered out using a solid-liquid separation procedure;finally,the material is dried and crushed.In order to evaluate its effects on the flammability of the EP,first,m-phenylenediamine is added to EP and vacuum defoamation is performed;then,EP is poured into a polytetrafluoroethylene mold,cooled to room temperature and demoulded;finally,the magnesium-based layered composite is added to EP,and its flame retardance is characterized by thermogravimetric analysis,limiting oxygen index and cone calorimetry.The X-ray diffraction patterns show that the baseline of magnesium-based layered composite is stable and the front shape is sharp and symmetrical when the molar ratio of magnesium to aluminium is 3.2:1;with the addition of magnesium-based layered composite,the initial pyrolysis temperature of EP of 10%,15%and 30%magnesium-based layered composite decreases to 318.2°C,317.9°C and 357.1°C,respectively.After the reaction,the amount of residual carbon increases to 0.1%,3.45%and 8.3%,and the limiting oxygen index increases by 28.3%,29.1%and 29.6%,respectively.The maximum heat release rate of cone calorimeter decreases gradually.The optimum molar ratio of Mg:Al for green synthesis is 3.2:1,and the NO_(3)-intercalated magnesium-based layered composite has the best flame retardance properties.
基金Financial support of the research project entitled "Enhanced Flame Retardant Polymer Nanocomposites" has been provided by Military Technical College,Cairo,Egypt
文摘Aluminum-oxide-hydroxide （AIOOH） is a clean and non-toxic flame retardant. There have been many trials for the fabrication of ultrafine AIOOH, Two main approaches exist for nano-AlOOH synthesis： reactive precipitation and batch hydrothermal synthesis, Both approaches are laborious and time consuming with poor control of particle morphology. We report on the novel continuous flow manufacture of AIOOH nanorods with controlled morphology （particle size and shape） by hydrothermal synthesis. AIOOH was harvested from its mother liquor （colloidal solution） using poly（acrylamide-co-acrylic acid） copolymer as a flocculating agent. The developed AIOOH shape and size, crystalline phase, thermal stability, and endothermic heat sink action were investigated by transmission electron microscopy, X-ray diffractome- try, thermogravimetric analysis, and differential scanning calorimetry, respectively. The phase transition of AlOOH to Al2O3 was demonstrated by conducting different X-ray diffractometry scans from 400 to 700℃. These results may provide an option for the continuous synthesis of nano-AIOOH as a clean and non-toxic flame retardant with excellent thermal stability. Consequently, enhanced flammability properties can be achieved at low solids loading.
基金Financial support of the research project entitled "Enhanced Flame Retardant Polymer Nanocomposites" has been provided by the Egyptian Military Technical College,Cairo,Egypt
文摘Nanoparticles can provide flame retardance to hosting polymers and act as nano fire extinguishers. Hydroxyapatite （Ca5（OH）（PO4）3） （HA） is not hygroscopic, and is thermally stable up to 800℃, with 18.5 wt% phosphorous content. It is this high phosphorous content that can provide HA with flame retardant properties. In this paper, we report on the continuous synthesis of ultrafine HA using a hydrothermal synthesis technique. The HA surface properties were changed from hydrophilic to hydrophobic by post-synthesis surface modification. The ratio of the HA nanoparticles and an intumescent agent known as Exolit AP750 was investigated to yield a self-extinguishing multi-component epoxy nanocomposite for extended application under extreme fire conditions. The HA/AP750/epoxy nanocomposite was able to resist a flame at 1700 oc and self-extinguish after the flame had been removed. The nanocomposite showed an enhanced flammability performance in standard cone calorimetry testing and formed a compact and cohesive protective char layer with a 50% decrease in peak heat released compared with virgin epoxy. Our aim was to establish the use of HA as an effective nanofiller with phosphorous-based flame retardant properties. The surface of this nano fire extinguisher was modified effectively with different surfactants for enhanced compatibility with different polymeric matrices.
文摘Red phosphorus （RP） has attracted considerable attention as the anode for high-performance Na-ion batteries, owing to its low cost and high theoretical specific capacity of -2,600 mAh/g. In this study, a facile single-step flash-heat treatment was developed to achieve the reduction of graphene oxide （GO） and the simultaneous deposition of RP onto the reduced graphene oxide （rGO） sheets. The resulting RP/rGO composite was shown to be a promising candidate for overcoming the issues associated with the poor electronic conductivity and large volume variation of RP during cycling. The RP/rGO flexible film anode delivered an average capacity of 1,625 mAh/g during 200 cycles at a charge/ discharge current density of 1 A/g. Average charge capacities of 1,786, 1,597, 1,324, and 679 mAh/g at 1, 2, 4, and 6 A/g current densities were obtained in the rate capability tests. Moreover, owing to the RP component, the RP/rGO film presented superior flame retardancy compared to an rGO film. This work thus introduces a highly accessible synthesis method to prepare flexible and safe RP anodes with superior electrochemical performance toward Na-ion storage.
基金financially supported by the Fundamental Research Funds for the Central Universities (No.2572014EB06-02)National Natural Science Foundation of China (No.51673035)Heilongjiang Major Research Projects (No.GA15A101)
文摘A phosphorus-nitrogen containing flame retardant additive of poly（phosphoric acid piperazine）, defined as PPAP, was synthesized by the salt-forming reaction between anhydrous piperazine and phosphoric acid, and the dehydration polymerization under heating in nitrogen atmosphere. Its chemical structure was well characterized by Fourier transform infrared（FTIR） spectroscopy, ^（13）C and ^（31）P solid-state nuclear magnetic resonance measurements. The synthesized PPAP and curing agent m-phenylenediamine were blended into epoxy resin（EP） to prepare flame retardant EP thermosets. The effects of PPAP on the fire retardancy and thermal degradation behavior of cured EP/PPAP composites were investigated by limiting oxygen index（LOI）, vertical burning（UL-94）, thermogravimetric analysis/infrared spectrometry（TG-IR） and cone calorimeter tests. The morphologies and chemical compositions of char residues for cured epoxy resin were investigated by scanning electron microscopy（SEM） and X-ray photoelectron spectroscopy（XPS）, respectively. The results demonstrated that the flame retardant EP thermosets successfully passed UL-94 V-0 flammability rating and the LOI value was as high as 30.8% when incorporating 5 wt% PPAP into the EP thermosets. The TGA results indicated that the synthesized PPAP flame retardant additive possessed high thermal stability and excellent charring capability. Meanwhile, the incorporation of PPAP stimulated the epoxy resin matrix to decompose and charring ahead of time due to its catalytic decomposition effect, which led to a higher char yield at high temperature. The morphological structures and the analysis results of XPS for char residues of EP thermosets revealed that the introduction of PPAP benefited the formation of a sufficient, more compact and homogeneous char layer containing phosphorus-nitrogen flame retardant elements on the material surface during combustion. The formed char layer with high quality effectively prevented the heat transmission and diffusion, limited the production of combustible gases, and inhibited the emission of smoke, leading to the reduction of heat and smoke release.
文摘Eight dialkyl tetrabromophthalates (DATBPs) were synthesized by reacting tetrabromophthalic anhydride with excess alcohols which were used not only as a reactant but also as a solvent and using a quaternary ammonium salt as a phase transfer catalyst (PTC). The yields were found to be between 85-93%. Their structures were characterized by IR, NMR and elementary analysis. The flame retardant properties of the compounds were also studied.
文摘Some organoboron compounds as flame-retardants for fiber materials were prepared.Flame-retarding properties of these compounds determined by the Oxygen-Index Method weregood.These new compounds were characterized by IR,~1H NMR spectrum and elementalanalysis.
文摘The synthesis, properties and flame retardation of two kinds of flame retardants, mono(1 chloride 2 hydroxy propyl) phosphate and antimony mono(1 chloride 2 hydroxy propyl)phosphate were reported. Mono(1 chloride 2 hydroxy propyl) phosphate was synthesized from epichlorohydrin and phosphoric acid at molar ratio of 1∶1.2 in the solvent of methyl benzene with AlCl 3 catalyst under the conditions of reaction temperature of 90 ℃ and reaction time of 2 h, its total yield is 82.5%. Antimony mono(1 chloride 2 hydroxy propyl)phosphate was synthesized from mono(1 chloride 2 hydroxy propyl)phosphate and antimony trioxide in the solvent of dimethyl sulfoxide with oxalic acid catalyst under the conditions of reaction temperature of 92 ℃ and reaction time of 4 h, the total yield is 85.6%. The physical chemical properties of the products were determined. When adding 15% of mono(1 chloride 2 hydroxy propyl) phosphate and antimony mono(1 chloride 2 hydroxy propyl)phosphate in polyethylene respectively, the oxygen indexes (OI) are 31.4 and 33.7 respectively. [
