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Synthesis And Application Of Organic Cage-like Phosphorus-nitrogen Synergistic Flame Retardant

Posted on:2019-08-04Degree:MasterType:Thesis
Country:ChinaCandidate:X LuoFull Text:PDF
GTID:2431330566483779Subject:Applied Chemistry
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Most polymer materials are flammable,causing huge property damage and casualties when the fire breaks out.In order to address the issues that polymer materials are flame retardant,the flame retardant properties of polymer materials are given.organic caged phosphorus-nitrogen synergistic flame retardant is halogen-free efficient and environmentally friendly flame retardant combining acid source,carbon source and gas source.Such inturnescent flame retardant are endowed with thermal insulation,oxygeninsulation and the prevention of droplet generation,which makes PU have good flame retardant properties.That's why organic caged phosphorus-nitrogen synergistic flame retardant is favored by researchers.In this paper,BPOD-PEPA wassynthesized from1-oxo-4-hydroxymenthyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane?PEPA?and Phenylphosphonic dichloride.In addition,Aniline and 2-Aminopyridine were reacted with BPOD-PEPA to produce synthesized BPOD-PEPA-A and BPOD-PEPA-AP.We studied synthesis conditions and application of flame-retardant polyurethane.As a intermediate of caged phosphorous-halgon,BPOD-PEPA wassynthesized from PEPA and Phenylphosphonicdichloride.Optimum reaction condition of BPOD-PEPA was Obtained as follow:n?BPOD?:n?PEPA?=1.7:1,The dropping time of PEPA solution of 50?was 3h,Volume ratio of 1,4-dioxane and acetonitrile was 3:1,magnetic speed was 800r/min,then heated 80?under reflux for 8h,the yield of BPOD-PEPA was 74.92%.and the structure was characterized by FT-IR,Elemental analysis,1H NMR and 31P NMR,The product obtained is the target sample BPOD-PEPA.the thermal properties were characterized by TGA,it proved that had good thermal stability and high residual carbon content,and is a better intermediate.Aniline and 2-Aminopyridine were reacted with BPOD-PEPA to produce synthesized BPOD-PEPA-A and BPOD-PEPA-AP.Under optimal process conditions,the yields of BPOD-PEPA-A and BPOD-PEPA-AP were 88.12%and 85.47%.and the structure was characterized by FT-IR,Elemental analysis,1H NMR and 31P NMR.the thermal properties were characterized by TGA,it proved that they had high residual carbon content,BPOD-PEPA-A had good thermal stability,but BPOD-PEPA-AP had general thermal stability.Their residual carbon morphologywas characterized by SEM and EDS,Carbon surface of BPOD-PEPA-A was dense and swollen without bubble.,but Carbon surface of BPOD-PEPA-AP was cracked and porous.Compared with the PU,BPOD-PEPA-A and BPOD-PEPA-AP flame-retardant PU have some effects,especially BPOD-PEPA-AP,The carbon residue of10%BPOD-PEPA-AP/PU and PU is 36.58%and 26.96%respectively,which is 9.62%higher than that of pure PU,Compared with the carbon residue of pure PU,it increases 9.62%?Combustionperformance of 10%BPOD-PEPA-AP/PU was lower than pure PU.and theTHR of 5%APP+5%BPOD-PEPA-AP/PU reduced by 65%than pure PU,It shows that BPOD-PEPA-AP and APP have certain synergistic flame retardant effect.
Keywords/Search Tags:cage, organic phosphorus-nitrogen synergistic flame retardant, flame retardant, thermal properties, combustion performance
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