Studies On The Synthesis, Crystal Structure And The Intumescent Flame Resistance Of Phosphorus, Silicone And Nitrogen Containing Compounds

The composite materials are widely used nowadays and their safety are much more concerned At the same time the need of flame retarded materials and flame retardant grows rapidly. Though the classical halide fire retarding agents have good performance.most of them give off heavy smoke with poisonous gas when burning. The flame retardants is developing toward high effective, no halogen, and light smoke in next years.Many traditional flame retardants are in a dilemma due to the more and more strict requirement of less smoke and less poisonous, which, however, offers a good opportunity for the development of the intumescent flame retardant(IFR) owing to its low smoke and low poison characteristics,and IFR has becoming one of the most active research fields and one of the most promising approach to realizing the accomplishment of research on non-halogen flame retardant.The intumescent flame retardant is composed by carbon source,acid source and gas source.The fire retardant element are Phosphorus and Nitrogen. When the flame retarded materials composed by these compounds are burned. The intumescent layer can insulate thermal N inhibit smoke and prevent producing molten drop ,so the flame retarding performance is high.Therefore, we design and synthesize 37 novel compounds that have never been Reported in any literature;①5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinansubstituted pyridylamine;②N-aroyl-N' -(-4-substituedphenyl(hydrogen)-5,5-dimethyl-1,3,2-dioxaphoryl)amino thioure;③N,N-aminopropyl-silatrane-benzyl-a-amino-5,5-dimethyl-4-substitued phenyl(hydrogen)-2-oxo-1,3,2-dioxaphosphorinane phosphonate;④ Spirocyclic Pentaerythritol Phosphorodichloridates.The reaction conditions and after-treatment process are studied and improved. The structure of the target compounds are confirmed by IR, 1HNMR, MS and elementary analysis. The spectroscopy properties are analyzed systematically. Result shows that the structures of the synthesized compounds are identical with the expected ones.TG and DSC analysis of some of the typical compounds are discussed. Most of the compounds begin to decompose at 200 ℃ and have certain thermal stability. They decompose rapidly during 200-400 ℃ and overlap many high polymer materialsdecomposition temperature range and show good fireproofing performance with materials.The high carbon residues at 600°C, which shows that the compounds have good carbonization function.We apply the compounds to alkyd resin varnish and epoxy resin(E-44) to test their flame resistanc. Among the many methods the level combustion method (GB2408-80) is used in epoxy resin as the standard. Result indicates that the title compounds have better flame resistance capability. The compounds I have the effect of self-extinguish within Is or 2s when 1% of them are added to alkyd resin varnish. All title compounds have the effect of self-extinguish with 10% of the total amount of the compounds I added to epoxy resin(E-44), and the combustion length is about 10~20mm in the level combustion test. Compounds IHandlV have better flame retardance than compounds I and II in epoxy resin(E-44). The samples foam and expand during the combustion process, and they carbonize and extinguish right after being deviated from fire, without melting and dropping and with low smoking. The thesis also gives a brief description of flame-retarding mechanisms and discusses the influence of the factor, such as P%,Si% and the existence of aromatization carbon on flame retardance.The above thermal analysis and initial fireproofing test show that the target compounds do have better flame retardance and are promising flame retardants.