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Preparation method of flame retardant trihydroxymethylphosphine oxide caged phosphite compound

A technology of trimethylol and phosphite, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the safety hazards of toxic gases and smoke, and halogen flame retardants Problems such as limited application range, to achieve the effect of good symmetry of the cage ring structure, easy large-scale transformation and production, and good flame retardancy

Active Publication Date: 2017-08-29
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the largest amount of halogenated flame retardants in my country is halogenated flame retardants. Although they have significant advantages, the toxic gases and smoke generated during combustion also have a large number of safety hazards. With the promulgation of some flame retardant laws by EU countries, halogenated flame retardants The scope of application of flame retardants is limited

Method used

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  • Preparation method of flame retardant trihydroxymethylphosphine oxide caged phosphite compound
  • Preparation method of flame retardant trihydroxymethylphosphine oxide caged phosphite compound
  • Preparation method of flame retardant trihydroxymethylphosphine oxide caged phosphite compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, the air in the bottle was driven away with nitrogen, and 30ml of acetonitrile, 14.00g (0.1 mol) trihydroxymethyl phosphine oxide, cooled to below 0°C, add 13.73g (0.1mol) phosphorus trichloride dropwise under stirring, make it fully mixed, heat up to 10°C, hydrogen chloride begins to be released, heat up to 25°C Keep warm for 1 hour, then raise the temperature to 80°C and keep warm for 3 hours. After no hydrogen chloride is released, remove acetonitrile by distillation under reduced pressure (for recycling), then add 50ml of ice water, and add 5% sodium carbonate solution dropwise under stirring to make the pH of the reaction system = 7. The product solid was dispersed in water, filtered, the filter cake was rinsed with 10 ml of ice water, compacted and drained, and the fil...

Embodiment 2

[0026] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, use nitrogen to exhaust the air in the bottle, add 40ml of benzene, 14.00g (0.1 mol) trihydroxymethyl phosphine oxide, cooled to below 0°C, add 13.73g (0.1mol) phosphorus trichloride dropwise under stirring, make it fully mixed, heat up to 10°C, hydrogen chloride begins to be released, heat up to 25°C Keep warm for 1 hour, then heat up to 75°C and keep warm for 4 hours. After no hydrogen chloride is released, benzene is removed by distillation under reduced pressure (recycled), then add 45ml of ice water, and add 5% sodium carbonate solution dropwise under stirring to make the reaction system pH= 7. The product solid was dispersed in water, filtered, the filter cake was rinsed with 10 ml of ice water, compacted and drained, and the filter cake was vacuum-dried to obtain a...

Embodiment 3

[0027] Example 3 In a 150ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, the air in the bottle was driven away with nitrogen, and 50ml of tetrahydrofuran was added, 14.00g (0.1 mol) trihydroxymethyl phosphine oxide, cooled to below 0°C, add 13.73g (0.1mol) phosphorus trichloride dropwise under stirring, make it fully mixed, heat up to 10°C, hydrogen chloride begins to be released, heat up to 25°C Keep warm for 1 hour, then raise the temperature to 65°C and keep it warm for 5 hours. After no hydrogen chloride is released, distill under reduced pressure to remove tetrahydrofuran (recycled), then add 40ml of ice water, add 5% sodium carbonate solution dropwise under stirring, and make the pH of the reaction system = 7. The product solid was dispersed in water, filtered, the filter cake was rinsed with 10 ml of ice water, compacted and drained, and ...

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Abstract

The invention relates to a method for preparing a fire retardant tris (hydroxymethyl) phosphine oxide caged phosphite ester compound. Please refer to the specification for the structural formula of the compound. According to the preparing method, phosphorus trichloride and tris (hydroxymethyl) phosphine oxide which are equimolar are sufficiently and evenly mixed at a temperature below 0 DEG C under the protection of nitrogen, temperature is increased to 25 DEG C and stays for 1 h, then temperature is increased to 60-80 DEG C and stays for 3-7 h for reaction, hydrogen chloride is drained, and then tris (hydroxymethyl) phosphine oxide caged phosphite ester is obtained through purification. The compound is high in phosphorus content, excellent in fire retardance, and suitable for serving as the fire retardant of materials including polyester, polyurethane, epoxy resin, unsaturated polyester resin and polyolefin. Furthermore, the preparing method is realized through one-step reaction, technique is simple, equipment investment is low, and industrial production is facilitated.

Description

technical field [0001] The invention relates to a preparation method of an organic phosphine flame retardant trimethylolphosphine oxide caged phosphite compound, in particular to a 4-oxo-2,6,7-trioxa-1,4-diphosphorous The invention discloses a preparation method of a heterobicyclo[2.2.2]octane compound, which is suitable for use as a flame retardant for materials such as polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and the like. Background technique [0002] In recent years, organic synthetic polymer materials have been widely used in various fields of the national economy, and the fires caused by them have seriously threatened the safety of people's lives and properties. Adding flame retardants to polymer materials to modify flammable polymer materials into flame-retardant materials is an effective means to prevent or reduce fires, thus promoting the rapid development of flame retardants. At present, the largest amount of halogenated flame retardants...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5397C08L67/02
Inventor 王彦林杨珂珂
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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