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Preparation method of flame retardant bisphosphoryl caged phosphate compound

A bisphosphoryl caged phosphate compound technology, which is applied in the field of preparation of organic phosphine flame retardant bisphosphoryl caged phosphate compounds, can solve problems such as restrictions on the use of halogenated flame retardants, and achieve cage ring structure symmetry Good performance, high flame retardant efficiency, easy operation

Active Publication Date: 2017-07-18
广州布司曼化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the European Union promulgated the RoHS directive in 1986, the use of halogenated flame retardants has been restricted

Method used

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  • Preparation method of flame retardant bisphosphoryl caged phosphate compound
  • Preparation method of flame retardant bisphosphoryl caged phosphate compound
  • Preparation method of flame retardant bisphosphoryl caged phosphate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 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, the air in the bottle was exhausted with nitrogen, and 30ml of dioxane was added, 14.00 g (0.1mol) trishydroxymethylphosphine oxide, cooled to below 10°C, add 15.33g (0.1mol) phosphorus oxychloride dropwise under stirring, make it fully mixed, heat up to 25°C, hydrogen chloride begins to be released, heat up Keep warm at 40°C for 2h, then raise the temperature to 100°C and keep warm for 4h, wait until no hydrogen chloride is released, remove dioxane by distillation under reduced pressure (for recycling), then add 50ml of ice water, add 5% sodium carbonate solution dropwise under stirring , the pH of the reaction system=7, the product solid was dispersed in water, filtered, the filter cake was rinsed with 10ml ice water, compacted and drained, the filter cake was vacuum-dr...

Embodiment 2

[0027] Embodiment 2 In the 100ml four-necked flask that stirrer, thermometer, high-efficiency reflux condensing tube are equipped with and being connected with hydrogen chloride absorption device on the condensing tube upper mouth, drive away the air in the bottle with nitrogen, add 40ml propionitrile, 14.00g ( 0.1mol) trishydroxymethyl phosphine oxide, cooled to below 10°C, add 15.33g (0.1mol) phosphorus oxychloride dropwise under stirring, make it fully mixed, heat up to 25°C, hydrogen chloride begins to be released, heat up to 40 ℃ for 2 hours, and then heated to 95 ℃ for 5 hours. After no hydrogen chloride is released, propionitrile is removed by distillation under reduced pressure (recycled), and then 45ml of ice water is added. With stirring, 5% sodium carbonate solution is added dropwise to make the reaction system pH=7, the product solid was dispersed in water, filtered, the filter cake was rinsed with 10ml of ice water, compacted and drained, and the filter cake was va...

Embodiment 3

[0028] 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 exhausted with nitrogen, and 50ml of dichloroethane was added, 14.00 g (0.1mol) trishydroxymethylphosphine oxide, cooled to below 10°C, add 15.33g (0.1mol) phosphorus oxychloride dropwise under stirring, make it fully mixed, heat up to 25°C, hydrogen chloride begins to be released, heat up Keep warm at 40°C for 2h, then raise the temperature to 85°C and keep warm for 6h. After no hydrogen chloride is released, dichloroethane is removed by distillation under reduced pressure (recycled), then add 55ml of ice water, and add 5% sodium carbonate solution dropwise under stirring. , the pH of the reaction system=7, the product solid was dispersed in water, filtered, the filter cake was rinsed with 10ml of ice water, compacted and drained, the filter cake ...

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Abstract

The invention relates to a preparation method for a flame retardant bisphosphoryl caged phosphate compound. The structure of the compound is as shown in a formula in the specification. The preparation method comprises the steps of: under the protection of nitrogen gas, sufficiently and uniformly mixing equimolar trihydroxymethyl phosphine oxide and phosphorus oxychloride at a temperature equal to or lower than 10 DEG C; heating the mixture to 40 DEG C and preserving the temperature for 2 hours; then, heating the mixture to 80-100 DEG C and preserving the temperature to react for 4-8 hours; exhausting hydrogen chloride; and carrying out purification to obtain the bisphosphoryl caged phosphate. The compound is high in phosphor content and excellent in flame retardant property, and is suitable for being used as the flame retardant of polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and the like. Moreover, the production process is simple; the equipment investment is low; the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of an organic phosphine flame retardant bisphosphoryl cage phosphate compound, in particular to a 1,4-dioxo-2,6,7-trioxa-1,4-diphospha The preparation method of the bicyclo[2.2.2]octane compound is suitable for use as a flame retardant for polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and other materials. Background technique [0002] In recent decades, due to the widespread application of flammable polymer materials, the fires caused by them have posed a huge threat to people's lives and property safety, thus promoting the promulgation and implementation of flame retardant regulations, and flame retardant technology has also been greatly improved. fast development. Currently widely used flame retardants include halogen-based, phosphorus-based and inorganic flame retardants. Halogenated flame retardants have been popular products in the field of flame retardants since the 1960s. The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5357C08K5/3492C08L67/02
Inventor 王彦林杨珂珂
Owner 广州布司曼化工科技有限公司
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