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Cyclic phenyl phosphonate compound and method for preparing same

A technology for phenylphosphonates and compounds, applied in the field of compound synthesis, can solve the problems of limited expansion, easy solubility of flame retardants in water, low thermal stability of flame retardants, etc., and achieves improved thermal stability and reaction steps. And the requirements of the reaction equipment are simple and inexpensive

Inactive Publication Date: 2012-09-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1888013A describes a bicyclic phosphate flame retardant, which uses pentaerythritol and dimethyl methylphosphonate or diethyl methylphosphonate, and has a higher phosphorus content in the product flame retardant. The flame retardant It is solid at room temperature, has good thermal stability and good compatibility with polymers, but the flame retardant is easily soluble in water
However, the flame retardant has low thermal stability and is easily soluble in water, which limits its application in engineering plastics and other fields.

Method used

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  • Cyclic phenyl phosphonate compound and method for preparing same
  • Cyclic phenyl phosphonate compound and method for preparing same
  • Cyclic phenyl phosphonate compound and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 134.17 g of trimethylolpropane, 124.08 g of trimethyl phosphite, and 2.5 g of triethylamine into a four-necked flask equipped with a stirrer, an atmospheric distillation device, a thermometer, and an air duct, and heat and stir to raise the temperature to 60°C , after the reaction time was 8 hours, rectification obtained 140.37g cage-shaped phosphoric acid ester intermediate. In the second step, 293.67g of triphenyl phosphite was added to the intermediate, and it was heated up to 150°C. After 15 hours of reaction, 376.60g of cyclic phenylphosphonate compounds were obtained. The reaction yield was 90%. The product structure is as follows:

[0020]

Embodiment 2

[0022] Add 134.17g of trimethylolpropane, 136.49g of trimethyl phosphite, and 0.8g of tetramethylammonium chloride into a four-necked flask equipped with a stirrer, an atmospheric distillation device, a thermometer, and an air duct, and heat and stir Raise the temperature to 70°C, the reaction time is 8 hours, and rectify to obtain 143.49g of the intermediate cage-shaped phosphate. In the second step, add 300.19g of triphenyl phosphite to the intermediate, and raise its temperature to 160°C, and the reaction time is After 16 hours, obtain 389.25g cyclic phenyl phosphonate compound, its productive rate is 91%, the chemical structural formula that obtains product is as follows;

[0023]

Embodiment 3

[0025] Add 134.17 g of trimethylolpropane and 148.90 g of trimethyl phosphite in a four-necked flask equipped with a stirrer, an atmospheric distillation device, a thermometer and an air duct, add 2 g of anhydrous aluminum trichloride, heat and stir to 80°C, the reaction time is 9 hours, rectification to obtain 155.97g of the intermediate cage-shaped phosphate ester. In the second step, 326.29g of triphenyl phosphite is added to the intermediate, and the mixture is heated to 170°C, and the reaction time is 16 Hour, obtain 437.04g cyclic phenyl phosphonate compound, its productive rate is 94%, obtain the chemical structure of product as follows:

[0026]

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Abstract

The invention relates to a cyclic phenyl phosphonate compound and a method for preparing the same, and in particular relates to a cyclic phenyl phosphonate compound having high thermal stability and hydrolysis resistance and a method for preparing the same. The structure of the compound provided by the invention is as shown in the specification, wherein n=0 or 1. The method provided by the invention is to synthesize the compound by a two-step method from trimethylolpropane, trimethyl phosphite and phosphorous acid. The compound is high in phosphorus content, low in toxicity, free of pollution and the like. With a benzene ring and a cyclic structure in the molecular structure, the thermal stability and hydrolysis resistance of the compound are greatly improved; and simultaneously, with the structure of the cyclic phosphonate and high phosphorus content in the molecular structure, the compound shows excellent flame retardant efficiency and can be widely applied to most flame retardant high molecular materials. Furthermore, the compound is rich in synthesis raw material source, simple in production process, and easy for realizing industrial production and application.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and relates to a cyclic phenylphosphonate compound and a preparation method thereof, in particular to a novel cyclic phenylphosphonate compound which can be used for polymer flame retardancy and a preparation method thereof. The invention relates to a cyclic phosphoric acid condensate containing a C-P bond and a benzene ring and a preparation method thereof. Background technique [0002] Since the 1950s, the use of polymer materials has become more and more extensive, and the amount of use has increased rapidly. The resulting fire hazard is greater, resulting in higher and higher requirements for the flame retardancy of polymer materials. In recent years, with the increase of people's awareness of environmental protection, halogen flame retardants have gradually withdrawn from the historical stage, and the demand for non-halogenated flame retardants has become higher and higher, and ph...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5357
Inventor 彭治汉惠银银吴迪游丽华邵偲淳
Owner DONGHUA UNIV
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