Esters Flame Retardants. Polycyclic Phosphine (phosphorus) Synthesis And Application Of Research

Along with expanding the scope of application of polymer materials, Increasingly strict fire prevention safety standards and human to protect the ecological environment and their own health are highly valued, flame retardants put forward higher and more comprehensive requirements, So for low smoke, non-halogen, high heat resistance, low toxicity and flame retardant of environmental protection has become the development direction.Cyclic phosphonate ester flame retardant is just about accord with development demand. This paper synthesized bicycle-phosphite ester intermediate by the ester exchange,cyclic phosphonate ester flame retardant was synthesized from the intermediate and phosphate,by the step of Arbuzov-Michaelis,the effects of process parameters,such as molar ratio,reaction temperature,reaction time and catalyst on the yiled were studied respectively.The suitable synthesis conditions were defined as follows:In the first step, the reaction temperature was 80～85℃, the reaction time was 12 hours, the reactant proportion of Trimethyl Phosphite and Dipentaerythritol was 2.3:1, the sutible catalyst was triethylamine, its dosage was 1.5% of the amount of all reactant; Similarly, the reaction temperature was 100～110℃, the reaction time was 10 hours, the reactant proportion of Triphenyl phosphite and Dipentaerythritol was 2.06:1, the sutible catalyst was sodium hydroxide, its dosage was 1.0% of the amount of all reactant.In the second step, for Phosphonic acid ester DTMP, the reaction temperature was 180～190℃, the reaction time was 16 hours, the reactant proportion of trimethyl phosphate and intermediate product was 1.5:1; for Phosphonic acid ester DTEP, the reaction temperature was 190～200℃, the reaction time was 15 hours, the reactant proportion of triethyl phosphate and intermediate product was 1.6:1; for Phosphonic acid ester DDMMP, the reaction temperature was 160～170℃, the reaction time was 18 hours, the reactant proportion of Dimethyl methylphosphonate and intermediate product was 1.6:1. The structure of the final compounds and the intermediate were confirmed by IR,1HNMR, and element analysis, and the heat stability was analyzed by TGA.On the base of reference bibliography, the application of Cricoid phosphonate ester, DDMMP flame retardant in PA6 and pure Dacron was studied, the result showed that it is a good flame retardant. The optimal amount and treatment conditions of flame retardant were obtained after the test and analysis of fire retardancy performance and mechanical performance of materials dealed with different amount and conditions and treatment conditions of flame retardant. The results showed that the LOI value of PA6/4% phosphonate ester, DDMMP/11% Melamine system was 28.8, the UL-94 test was V-0 level; Study on Flame Finish of Polyester Fabric showed that the pH value should be adjusted to 6～6.5, the curing temperature was 180～185℃, the use level of flame retardant was 110 g/L, the flame retardancy met B1 grade of national standard.