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Method for synthesizing monomolecular phosphorus-nitrogen expansion type fire retardant

A synthesis method and single-molecule technology, applied in the direction of phosphorus organic compounds, etc., can solve the problems of poor compatibility between flame retardants and materials, complex single-molecule IFR process, environmental pollution, etc., to achieve good compatibility and protect physical and mechanical properties. , the effect of low price

Inactive Publication Date: 2008-04-30
SHUNDE POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the deficiencies in the prior art, proposes a kind of preparation method of monomolecular phosphorus-nitrogen intumescent flame retardant, to overcome the poor compatibility of flame retardant and material in the prior art; Use halogen-containing flame retardant to cause Environmental pollution and the complex and costly process of preparing single-molecule IFR

Method used

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  • Method for synthesizing monomolecular phosphorus-nitrogen expansion type fire retardant
  • Method for synthesizing monomolecular phosphorus-nitrogen expansion type fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 1.36g of pentaerythritol and 50ml of dioxane to a 250ml round bottom flask equipped with a nitrogen inlet and outlet, a drying device, a pear-shaped separating funnel, and a stirring device, stir well to dissolve the pentaerythritol, and use a pear-shaped separating funnel to dissolve the pentaerythritol. 1.53g of phosphorus oxychloride was added dropwise and reacted for 1h under stirring, a large amount of white precipitates were produced. Filter, wash twice with deionized water, then wash twice with acetone, and dry in vacuum for 24 hours to obtain a white powdery solid with a yield of 95%.

[0031] Add 3.60g of the white solid PEPA obtained from the above reaction into a 250ml round-bottomed flask equipped with a drying device, a pear-shaped separating funnel and a stirring device, add 100ml of DMF as a solvent, stir to dissolve the PEPA, and then add dropwise through the pear-shaped separating funnel 1.74g TDI, fully stirred, reacted for 2 hours, gradually a lig...

Embodiment 2

[0034] Add 2.72g of pentaerythritol and 150ml of dioxane to a 250ml round-bottomed flask equipped with a nitrogen inlet and outlet, a drying device, a pear-shaped separating funnel and a stirring device, stir well to dissolve the pentaerythritol, and use a pear-shaped separating funnel Add 3.06g of phosphorus oxychloride dropwise and react for 0.5h under stirring, a large amount of white precipitates are produced. Filter, wash twice with deionized water, then wash twice with acetone, and dry in vacuum for 24 hours to obtain a white powdery solid with a yield of 92%.

[0035] Add 3.60g of the white solid PEPA obtained from the above reaction into a 250ml round-bottomed flask equipped with a drying device, a pear-shaped separating funnel and a stirring device, add 100ml of DMF as a solvent, stir to dissolve the PEPA, and then add dropwise through the pear-shaped separating funnel 2. 50gMDI, fully stirred, reacted for 2h, a light yellow precipitate gradually formed, the product w...

Embodiment 3

[0037] Add 2.72g of pentaerythritol and 150ml of dioxane to a 250ml round-bottomed flask equipped with a nitrogen inlet and outlet, a drying device, a pear-shaped separating funnel and a stirring device, stir well to dissolve the pentaerythritol, and use a pear-shaped separating funnel 3.06g of phosphorus oxychloride was added dropwise and reacted for 5h under stirring, a large amount of white precipitates were produced. Filter, wash twice with deionized water, then wash twice with acetone, and dry in vacuum for 12 hours to obtain a white powdery solid with a yield of 96%.

[0038] Add 3.60g of the white solid PEPA obtained from the above reaction into a 250ml round-bottomed flask equipped with a drying device, a pear-shaped separating funnel and a stirring device, add 100ml of DMF as a solvent, stir to dissolve the PEPA, and then add dropwise through the pear-shaped separating funnel 2. 50g of MDI, fully stirred, reacted for 10 hours, a light yellow precipitate gradually form...

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Abstract

The invention relates to a method for synthesizing a monomolecular phosphorus-nitrogen expansion flame retardant, which is characterized by: reacting pentaerythritol and phosphorus oxychloride at 80-120°C for 2-12 hours, adding the first solvent during the reaction, and the reaction ends After cooling, filtering, washing, and vacuum drying for 12-24 hours to obtain a white solid, the white solid is 1-oxo-4-hydroxymethyl-1-phospho-hetero-2,6,7-trioxabicyclo [2, 2, 2] octane (PEPA); then add the white solid (PEPA) into the second solvent, stir rapidly to dissolve it, then add isocyanate substances dropwise, and add the catalyst dropwise at the same time, stirring continuously, the reaction The time is 1 to 12 hours, the reaction temperature is 20 to 100°C, the solution changes from clear to turbid, the product is poured into ice water, an appropriate amount of inorganic acid is added dropwise, the pH value is adjusted to be acidic, a white solid is precipitated, and then washed with a washing solvent for 3 The filtered product was vacuum-dried to obtain a white or light yellow solid with a yield of 90-96%. It has the advantages of no halogen, non-toxicity, environmental protection, good application prospects and the like.

Description

technical field [0001] The invention relates to the technical field of flame retardants and preparation methods thereof, in particular to a synthesis method of phosphorus-nitrogen intumescent flame retardants. technical background [0002] Flame retardant is one of the most important additives in the processing of polymer materials. Traditional flame retardants generally contain halogens. Although they have good flame retardant performance, such flame retardants will release a large amount of corrosive The application of toxic and toxic gases is limited in many fields, so there is a tendency to be gradually replaced. [0003] Phosphorus-nitrogen intumescent flame retardant (IFR) does not contain halogen, and mainly consists of phosphorus P, nitrogen N, and carbon C. When heated, the phosphorus-nitrogen complex effect in the molecule can occur to form a uniform and dense carbon layer. Adsorbs the polymer that melts and catches fire, prevents the dripping of the polymer from ...

Claims

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Application Information

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IPC IPC(8): C07F9/09C09K21/12
Inventor 刘洪波冯才敏张永雄
Owner SHUNDE POLYTECHNIC
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