酚氧基环三磷腈的合成及其在聚烯烃弹性体中的协同阻燃特性

研究快讯合成橡胶工业,2007-11-15,30(6):472CommunicatieCHINA SYNTHETIC RUBBER INDUSTRYSynthesis of phenoxy cyclotriphosphazene and its synergisticflame retardancy in polyolefin elastomerKong Xiangjian, Liu Shumei, Ye Hua, Zhao JianqingCollege of Materials Science and Engineering, South China University of Technology, Guangzhou 510640, China)In recent years, halogen-free flame-retardants such as metal hydron. different compositions. When PCP was added to the pure POE, Lolidem, organophosphate compounds, organosilicon derivativee have values increased only about 1%-2% with increasing mass fraction ofbeen used in polymeric aterials to avoid the generation of corrosi1%-2% of PCP in the system. When PCP was added to the cohalogenated gases[J. Halogen-free cyelotriphosphazene derivativespound, a synergism was observed, i. e., LOI values rap:dly increasedrich in both phosphorus and nitrogen, usually synthesized through the with the increase of PCP contents in the blends, POE/MH blends withnucleophilic substitution reaction of hexachlorocyclotriphosphazeness fraction of 2% PCP resulted in LOI values as high as 36%.Theattractive candidates as name- -retardant additives, However, the synergism was due to the enhanced condensed-phase retardation by thesynthesis processes of cyclophosphazene derivatives, such as phenoladdition of PCPsubstituted cyclotriphosphazene, are complicated, and the expensivewhere high reactive sodium or sodium hydride must be used in manyTabl 1 Flame retardant propertles of POE blendsadiwith different compositionsIn thim paper, sodium hydroxide was employed instead of sodiumMagg fraction of Mass fraction of Mass fraction ofsodium hydride, and the synthetie method was improved. PhenolD0%POE/%PCP/%MH/%(13.2 g)was dissoived in dry tetrahydrofuran(THF)and sodium hydroxide(5.6 g)was added to65 C under mechanical agitation. When the system tumed into theclearly yellow solution, hexachlorocyclotriphosphazene(8. 1 g)98dded. The system was kept agitated at 65 t for 48 h, the yellususpended solution0120120000890026cuum-distilled off and the residuewith cold waterremove unreacted sodium phenolate andAachloridelized in THF and dried at 60 C under vacuum for 24 h. The wpowderphenoxy cyclotriphoaphazene, PCP was obtainedReferencesI Yuan C Y, Chen S Y, TeaiC H, et al. Thermally stable andinfrred spectroscopy( IR)analytical results in Fig 1 indicatedfame-rctardant aromatic phosphate and cyclotriphoephazene-conoverall compositions of the product corresponded to the expetaining polyurethanes: Synthesia and properties[ J ] Polym Advon peaks atto P=N bonds. P-0-c bonds appeared ar y0 at-Technol,2005,16:393~3992 Mathew D, Reghunadhan Nair C P, Ninan K N, Phosphazene-tnions at 1 487 cm"and 1 591 cm-line eyclomatrix network polymen: Some aspects of synthesiswas due to the aromatic groups. Compared with the IR spectra of hexa-thermal and flame-retardant characteristics[ J], Polym Int,2000blorocyclotriphosphazene, the absorption peak at 601 em"(due toP-Cl bonds) disappeared酚氧基环三磷的合成及其在聚烯烃弹性体中的协同阻燃特性孔祥建,刘述梅,叶华,赵建青(华南理工大学材料科学与工程学院,广东广州510640)以苯酚与六氯环三磷腈为原料,氢氰化钠为催化剂,在四氢呋喃溶剂中直接合成了环三磷腈的苯酚取代物,避免了金属钠或NH的使用,合虎工艺简便而安全。将所合成的酚氧基环三磷腈与氢氧化镁复配用于聚烯烃弹性体的阻燃。结果表明,所合成的磷腈衍生物与氧氧化镁具有良好的协同阻燃作用,当体系中氢氧化镁的质量分数为4000350300252001500100048%,酚氧基环三磷腑质量分数为2%时,共混物的限氧Wavenumbericm'指数达到36%,具有良好的阻燃效果。关键词:酚氧基环三磷腈;合成;聚烯烃弹性体;协同阻燃Fig I IR spectra of PCPThe flame retardant polyolefin elastomer( POE )was obtained bypounding mass fraction of% PCP synthesized above,mRecelved: 2007-05-17.frction of 48%-50% magnesium hydroxide( MH)and maM frac-on of 50% POE in a mill mixer t 200-210 C. The limiting oxygex( Lol)value va determined using a flammability中国煤化工 cience Foundation ofade in Fire Testing Technology with standard specimens of siz-ets( Dongguan Spe-125 mm x6.5 mm x 3 mm sccording to GB/T 2406-1993.CNMHGTable 1 listed the LOl values of flame retardant Poe elastomer withTo who all correspondence should be addressed