Synthesis method of novel reactive bicyclophosphate flame retardant
A bicyclic phosphate ester and synthesis method technology, applied in the field of flame retardants, can solve the problems of low molecular weight, easy migration, low flame retardant efficiency, etc., achieve less smoke generation, simple synthesis process, and overcome low flame retardant efficiency Effect
Inactive Publication Date: 2017-08-18
ANYANG INST OF TECH
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Problems solved by technology
Among the halogen-free flame retardants, more and more people favor organophosphorus flame retardants with the characteristics of low toxicity, high efficiency, and environmental harmlessness. However, traditional organophosphorus flame retardants also have low molecular weight, Easy to move out, low flame retardant efficiency and other shortcomings, so improving the thermal stability and flame retardant efficiency of phosphorus flame retardants is one of its development directions
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[0019] This method comprises the following steps in turn:
[0020] 1. The synthesis of intermediate PDD: Add dichloromethane (50mL), 13.6g (0.1mol) of pentaerythritol, triethylamine ( 2mL), and 19.17mL (0.21mol) of phosphorus oxychloride was installed in a constant pressure dropping funnel. Stir and heat slowly, and slowly add phosphorus oxychloride dropwise when the temperature reaches 40°C. Use dilute sodium hydroxide solution to absorb the tail gas hydrogen chloride produced by the reaction. When the phosphorus oxychloride was added dropwise, the temperature was raised to 50°C to form a uniform suspension, and the time and phenomenon of the reaction was recorded. The temperature was controlled at 50°C and the reaction was continued for 6 hours before the reaction was stopped. The product was washed with washing solvents such as dichloromethane and absolute ethanol, multi-step suction filtration with a clean suction filter bottle, dried in a vacuum drying oven, and the rea...
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The invention provides a synthesis method of a novel reactive bicyclophosphate flame retardant. The optimal technological conditions for synthesizing the intermediate pentaerythritol bisphosphorate diphosphoryl chloride (PDD) from phosphorus oxychloride and pentaerythritol are as follows: a certain amount of dichloromethane is used as a solvent, a certain amount of triethylamine is used as an acid-binding agent, the mole ratio of the reactants pentaerythritol and phosphorus oxychloride is 1:2.1, the reaction temperature is 50 DEG C, and the reaction time is 6 hours. The optimal technological conditions for synthesizing the target product pentaerythritol bisphosphorate diphosphoryl chloride propenol salt (PDA) are as follows: the mole ratio of the reactants PDD and propenol is 1:2.2, and the reaction is carried out for 8 hours under ice bath conditions. The method has the advantage of simple technique, and is green and environment-friendly. The novel flame retardant synthesized by the method has the advantages of no halogen, no toxicity, high heat stability and the like, can well overcome the defects of low flame-retardant efficiency, high migration tendency, poor compatibility with high-molecular materials and the like in the additive-type phosphorus flame retardant, conforms to the environmental requirements which are advocated at present, and has wide development prospects.
Description
technical field [0001] The invention belongs to the technical field of flame retardants, and relates to a method for synthesizing a flame retardant, in particular to a method for synthesizing a novel reactive bicyclic phosphate flame retardant. Background technique [0002] Since the mid-20th century, with the rise of the petrochemical industry, natural and synthetic polymer materials have been widely used in all aspects of life due to their excellent comprehensive properties, light weight, and easy processing. The vigorous development of polymer materials has given people life has brought many conveniences. While enjoying the convenience brought by polymer technology, people are also suffering from serious hazards caused by the flammability of polymer materials, which threaten people's lives and property safety. Therefore, polymer materials are facing pressure from society and the environment regarding the flame retardancy requirements of materials. The introduction of fl...
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IPC IPC(8): C07F9/6574C08K5/527
CPCC07F9/65746C08K5/527
Inventor 王艳飞杨立国吕会超王鑫宋海香牛永生侯绍刚
Owner ANYANG INST OF TECH