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Phosphorus-nitrogen type flame retardant containing active double bond as well as preparation method and application thereof

A phosphorus-nitrogen-based flame retardant and active technology are applied in the field of phosphorus-nitrogen-based flame retardants and their preparation, which can solve the problems of flame retardant loss and product performance deterioration, and achieve good flame retardant effect, low cost, and easy industrialization. Effect

Active Publication Date: 2015-01-07
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For common thermoplastic materials such as polystyrene, polymethyl methacrylate, etc., most of them can only use additive flame retardants, but since most of the flame retardants used are still small molecules, this type of additive flame retardant products There is still the disadvantage that the performance of the product will deteriorate due to the loss and migration of the flame retardant during use

Method used

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  • Phosphorus-nitrogen type flame retardant containing active double bond as well as preparation method and application thereof
  • Phosphorus-nitrogen type flame retardant containing active double bond as well as preparation method and application thereof
  • Phosphorus-nitrogen type flame retardant containing active double bond as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 43.2 g (0.2 mol) of DOPO, 10.9 g (0.1 mol) of p-aminophenol, 6.0 g (0.1 mol) of paraformaldehyde and 200 mL of ethanol into a 500 mL three-necked round bottom flask, slowly raise the temperature to 50 °C and stir And reflux reaction for 5h, and then the crude product was obtained after the solvent was removed by rotary evaporation, and the phenolic intermediate compound was obtained after repeated washing with methanol three times and drying, with a yield of about 95%.

[0028] Add 33.2g (0.05mol) of the previously synthesized phenolic intermediate compound, 10.1g (0.10mol) of triethylamine and 100mL of dichloromethane to a 250mL single-necked round-bottomed flask in sequence, place it at 5°C, and slowly 10.5 g (0.10 mol) of methacryloyl chloride was added dropwise, and stirring was continued for 8 hours after the dropwise addition was completed. After the reaction was completed, triethylamine hydrochloride was removed by filtration, and washed several times with 3%...

Embodiment 2

[0030] Add 43.2 g (0.2 mol) of DOPO, 10.9 g (0.1 mol) of p-aminophenol, 6.0 g (0.1 mol) of paraformaldehyde and 200 mL of tetrahydrofuran into a 500 mL three-necked round-bottomed flask, slowly heat up to 65 °C and stir And reflux reaction for 4h, and then the crude product was obtained after the solvent was removed by rotary evaporation, and the phenolic intermediate compound was obtained after repeated washing with methanol three times and drying, with a yield of about 88%.

[0031]In a 250mL single-necked round bottom flask, add 33.2g (0.05mol) of previously synthesized phenolic intermediate compound, 10.1g (0.10mol) of triethylamine and 100mL of dichloromethane in sequence, place it at 20°C, and slowly 7.9 g (0.10 mol) of methacryloyl chloride was added dropwise, and stirring was continued for 6 h after the dropwise addition was completed. After the reaction was completed, pyridine hydrochloride was removed by filtration, and washed several times with 3% NaOH solution, dis...

Embodiment 3

[0033] Add 43.2 g (0.2 mol) of DOPO, 10.9 g (0.1 mol) of p-aminophenol, 6.0 g (0.1 mol) of paraformaldehyde and 200 mL of acetonitrile into a 500 mL three-necked round-bottomed flask, slowly raise the temperature to 80 °C and stir And reflux reaction for 3h, then the crude product was obtained after the solvent was removed by rotary evaporation, and the phenolic intermediate compound was obtained after repeated washing with methanol three times and drying, with a yield of about 92%.

[0034] Add 33.2g (0.05mol) of the previously synthesized phenolic intermediate compound, 10.1g (0.10mol) of triethylamine and 100mL of toluene to a 250mL single-necked round-bottomed flask in sequence, place it at 40°C, and slowly drop 10.5g (0.10mol) of methacryloyl chloride, after the dropwise addition, continue to stir and react for 4h. The back was washed several times with 3% NaOH solution, distilled water, and saturated NaCl aqueous solution successively. Anhydrous MgSO for organic layer ...

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Abstract

The invention discloses a phosphorus-nitrogen type flame retardant containing an active double bond as well as a preparation method and an application thereof. The preparation method comprises the following steps: carrying out Mannich reaction on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, p-aminophenol and paraformaldehyde in the presence of a solvent to obtain a product and washing the product with methanol to obtain a phenolic intermediate compound; reacting the phenolic intermediate compound with methacryloyl chloride in the presence of a solvent and an acid binding agent, filtering to remove acid binding agent salts generated in the reaction to obtain a crude product, purifying the crude product by virtue of washing, carrying out spin evaporation and drying to obtain the phosphorus-nitrogen type flame retardant containing the active double bond. The phosphorus-nitrogen type flame retardant containing the active double bond can be applied in preparation of flame-retardant polymer materials. The raw materials are easily available and the cost is low; the reaction conditions are mild and the yield is high; the purification and separation operations of the product are simple and the phosphorus-nitrogen type flame retardant is easily industrialized and complies with environmental requirements; the flame-retardant effect is good and the application range is wide.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a phosphorus-nitrogen flame retardant containing active double bonds, a preparation method and application thereof. Background technique [0002] Since the widespread use of organic synthetic polymer materials, human beings have begun to face new fire threats. The reason is that most of these materials are flammable or combustible. By adding flame retardants, the ignition of the material can be suppressed and the flame resistance of the material can be improved to prevent the material from burning and inhibit the flame from spreading. Traditional halogen-containing flame retardants are favored due to their excellent flame retardant effect, but they will emit toxic and corrosive gases during application, and the composite materials will produce a large amount of smoke, which will cause certain harm to the human body and the environment. The proposal of non-halogenation makes phosphorus-based ...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5313C08L33/12C08L25/06
Inventor 戴李宗陈国荣袁丛辉刘诚陈显明李远源罗伟昂何凯斌曾碧榕刘新瑜
Owner XIAMEN UNIV
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