Study On The Synthesis And Flame Resistance Of Derivatives Of 1, 3, 2-Dioxaphosphorinane

With the development of science technology, the application of polymeric materials has been on the rise and has involved almost every aspect of people's daily life. Accordingly, the fire disasters caused by then- combustion, which is a social problem that concerns all human beings and then- environment, have attracted more and more attention from people all over the world. Thus, it is of great significance to carry research on the treatment of inflammable materials with flame retardants, and to lay out reasonable flame retardant regulation and standard so as to improve people capability of preventing fire disasters and to reduce the loss caused by those disasters.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 inrumescent 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.Therefore, we design and synthesize 24 novel compounds that have never been Reported in any literature:(1)N,N-bis(5,5-dimethyl-4-aiyl-2-oxo(sul)-l,3,2-dioxaph osphacyclohexyl-2-)piperazine;(2)N,N'-bis(5,5-dunethyl-4-aryl-2-oxo(sul)-1,3,2-di oxaphosphacyclohexyl-2-)ethylene(promethylene,hexmethylene)diamine;(3)N,N'-bis(5,5-dimethyl-4-aryl-2-oxo(sul)-l,3,2-dioxaphosphacyclohexyl-2-)urea(thiourea ,imino-urea).The reaction conditions and after-treatment process are studied and improved. The structure of the target compounds are confirmed by IR, 1HNMR, 31NMR, 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 220℃ and have certain thermal stability.They decompose rapidly during 220-400℃ and overlap many high polymer materials decomposition temperature range and show good fireproofing performance with materials.The high carbon residues at 600℃, which shows that the compounds have good carbonization function.We apply the compounds to alkyd resin varnish, epoxy resin(E-44) to test their flame resistanc. Among the methods the level combustion method (GB2408-80) used in epoxy resin are standard methods. Result indicates that the title compounds have better flame resistance capability. The compounds I have the effect of self-extinguish within Is or 2s with 1% addition in alkyd resin varnish. All title compounds have the effect of self-extinguish with 10% addition in epoxy resin(E-44), and the combustion length is about 10~20mm in the level combustion test. Compounds I and II have better flame retardance than compounds III 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%,S% 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 m flame retardants.