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Phosphorus and nitrogen flame retardant and preparation method thereof

A phosphorus-nitrogen flame retardant and flame retardant technology, applied in the field of flame retardants, can solve problems such as environmental safety hazards and application restrictions, and achieve the effects of good flame retardant effect, simple production conditions and reduced dosage.

Inactive Publication Date: 2015-02-11
NANYANG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The application of traditional halogenated flame retardants, especially brominated flame retardants, has been continuously restricted due to environmental safety hazards in the combustion process.

Method used

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  • Phosphorus and nitrogen flame retardant and preparation method thereof
  • Phosphorus and nitrogen flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 2,2-dimethylol-3-nitro-1-propanol (16.51g, 0.1mol) into a 500ml three-neck flask equipped with a thermometer, a 100ml constant pressure dropping funnel, a magnet and an exhaust gas absorption device, Triethylamine (35.42g, 0.35mol) and 200ml chloroform, turn on the magnetic stirring, dissolve phosphorus trichloride (17.79g, 0.105mol) in 50ml chloroform, add to the constant pressure funnel, at 0~5℃, Slowly added dropwise to the three-necked flask. After the dropwise addition, the reaction was continued for 6 hours. After the reaction, the reactant was distilled, and the low boiling point solvent was recovered and recycled, while the high boiling point residue was washed with deionized water and filtered to obtain a solid that was vacuum dried at 40°C for 6 hours. Obtain 18.32 grams of white powdery phosphorus nitrogen flame retardant solid, yield 93%.

Embodiment 2

[0019] Add 2,2-dimethylol-3-nitro-1-propanol (16.51g, 0.1mol) into a 500ml three-neck flask equipped with a thermometer, a 100ml constant pressure dropping funnel, a magnet and an exhaust gas absorption device, Pyridine (27.69g, 0.35mol) and 200ml of dichloromethane, turn on the magnetic stirring, dissolve phosphorus trichloride (17.79g, 0.105mol) in 50ml of dichloromethane, add to the constant pressure funnel, at 0~5℃ Slowly drop it into the three-neck flask. After the dropwise addition, the reaction was continued for 6 hours. After the reaction, the reactant was distilled, and the low boiling point solvent was recovered and recycled, while the high boiling point residue was washed with deionized water and filtered to obtain a solid that was vacuum dried at 40°C for 6 hours. Obtain 18.81 grams of solid white powder phosphorus nitrogen flame retardant, yield 95%.

Embodiment 3

[0021] Add 2,2-dimethylol-3-nitro-1-propanol (16.51g, 0.1mol) into a 500ml three-neck flask equipped with a thermometer, a 100ml constant pressure dropping funnel, a magnet and an exhaust gas absorption device, Sodium carbonate (18.58g, 0.175mol) and 200ml acetonitrile, turn on the magnetic stirring, dissolve phosphorus trichloride (17.79g, 0.105mol) in 50ml acetonitrile, add to the constant pressure funnel, at 0~5℃, slowly Add dropwise to a three-neck flask. After the dropwise addition, the reaction was continued for 6 hours. After the reaction, the reactant was distilled, and the low boiling point solvent was recovered and recycled, while the high boiling point residue was washed with deionized water and filtered to obtain a solid that was vacuum dried at 40°C for 6 hours. Obtain 17.71 grams of white powdery phosphorus nitrogen flame retardant solid, yield 90%.

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Abstract

The invention discloses a phosphorus and nitrogen flame retardant and a preparation method thereof. A structural formula of the flame retardant is shown in the specification. The preparation method comprises the following steps: firstly dissolving 2,2-dihydroxymethyl-3-nitro-1-propanol and an acid-binding agent in a solvent and adding 2,2-dihydroxymethyl-3-nitro-1-propanol and the acid-binding agent to a three-neck flask, then dropping thiophosphoryl chloride, stirring the materials uniformly, regulating the temperature to 0-50 DEG C and carrying out thermostatic reaction for 5-8 hours, evaporating the solvent at reduced pressure after the reaction is completed, washing the residual solid with distilled water and filtering the residual solid, and carrying out vacuum drying on the product, thus obtaining the phosphorus and nitrogen flame retardant. The synthetic process is simple and is mild in conditions. Nitro functional groups in the molecules of the phosphorus and nitrogen flame retardant can be easily transformed to amino with higher activity, can serve as intermediates for developing novel flame retardants, more importantly, can directly react on polymers or raw materials of the polymers after being reduced to amino, and can be widely applied to the polymers of various base materials.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a phosphorus-nitrogen flame retardant and a preparation method thereof. The flame retardant can be used in coatings, adhesives, plastics, rubber and other fields requiring flame retardancy. Background technique [0002] At present, polymer materials are used more and more widely in people's lives, involving almost every aspect of life. However, fires caused by flammable polymer materials occur frequently, which poses a great threat to people's lives and property safety. How to reduce the combustion performance of polymer materials has become an increasingly concerned technical and social issue, which provides a broad market for the research and development of flame retardants. The application of traditional halogenated flame retardants, especially brominated flame retardants, has been restricted due to the environmental safety hazards in the combustion process. With t...

Claims

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Application Information

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IPC IPC(8): C08K5/5398C07F9/6574
Inventor 张群安杜朝军刘建连
Owner NANYANG INST OF TECH
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