Flame-retardant polystyrene/layered inorganic nanocomposite and preparation method thereof

Abstract

The invention relates to a flame-retardant polystyrene / layered inorganic nanocomposite and a preparation method thereof, which is characterized in that phenyl dichlorophosphate is taken as a reaction matrix for being reacted with polyol or polyphenol which is partially acrylated or partially methacrylated, and then the reaction with a nitrogen-containing compound with a reactive amino group is carried out, thereby obtaining the flame-retardant comonomer which simultaneously has an active double bond and a phosphorus-nitrogen flame-retardant element; the phosphorus-nitrogen monomer and styreneare used for preparing the flame-retardant polystyrene / layered inorganic nanocomposite through the free radical in-situ intercalation polymerization method in the presence of a layered inorganic; a phosphorus-nitrogen-containing flame retardant which is connected with a polymer molecular chain by the chemical bond way has better compatibility with a resin substrate and is more environment-friendly, and the flame retardant has no migration and no loss; the layered inorganic can further improve the thermal stability and the flame-retardant performance of a polymer substrate; and the flame-retardant polystyrene / layered inorganic nanocomposite can be directly prepared into a flame-retardant polystyrene material and can also be prepared into a flame-retardant masterbatch to be added in other plastics.

Description

technical field

[0001] The invention belongs to the technical field of flame-retardant polymer / layered inorganic compound, and in particular relates to a phosphorus-nitrogen-containing flame-retardant polystyrene / layered inorganic compound nano-composite and a preparation method thereof. Background technique

[0002] As one of the five general-purpose plastics, polystyrene (PS) has the advantages of excellent formability, hard quality, transparency, electrical insulation, low moisture absorption, easy dyeing and low price, and has been widely used in electronics, automobiles, construction, Toys, packaging and other industries. However, polystyrene is easy to burn and drips heavily when burning. These shortcomings limit its popularization and use in occasions with high fire protection requirements. At present, the flammability of polystyrene is usually solved by adding halogenated flame retardants or adding phosphorus-containing organic or inorganic compounds. However, thes...

Examples

Embodiment 1

[0026] In a 250ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) of phenyl phosphate dichloride and 80ml of tetrahydrofuran, stir in an ice bath at -5 to 5°C, and after 20 minutes, add 21.2 g (0.21 mol) of triethylamine, and slowly add a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of tetrahydrofuran dropwise within 2 hours under continuous stirring, and continue to react for 4 hours. Then, 7.32 g (0.1 mol) of diethylamine was dissolved in 80 ml of tetrahydrofuran, and slowly dropped into the above reaction system under the condition of ice bath at -5-5° C. under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the obtained light yellow transparent liquid is the product of the present invention. The yield was 80%.

[0027] The obtained product was analyzed ...

Embodiment 2

[0031] In a 250ml three-necked flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml methylene chloride, stir in an ice bath, and after 10 minutes, add 21.2g (0.21 mol) triethylamine, then slowly dropwise added a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of dichloromethane in 2 hours under continuous stirring, and continued to react for 4 hours. Then 7.32 g (0.1 mol) of diethylamine was dissolved in 60 ml of dichloromethane, and slowly dropped into the above reaction system under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the obtained light yellow transparent liquid is the product of the present invention. The yield was 85%.

[0032] The obtained product was analyzed by nuclear magnetic resonance spectrum. The peak position of th...

Embodiment 3

[0035] In a 250ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml tetrahydrofuran, stir in an ice bath, and after 10 minutes, add 21.2g (0.21mol) Triethylamine, and a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of tetrahydrofuran was slowly added dropwise within 2 hours under continuous stirring, and the reaction was continued for 4 hours. Then diethylamine was dissolved in 80ml of tetrahydrofuran, and slowly dropped into the above reaction system under continuous stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the obtained yellow transparent liquid is the product of the present invention. The yield was 80%.

[0036]The obtained product was analyzed by nuclear magnetic resonance spectrum. The peak position of the chemical shift ...

technical field

[0001] The invention belongs to the technical field of flame-retardant polymer / layered inorganic compound, and in particular relates to a phosphorus-nitrogen-containing flame-retardant polystyrene / layered inorganic compound nano-composite and a preparation method thereof. Background technique

[0002] As one of the five general-purpose plastics, polystyrene (PS) has the advantages of excellent formability, hard quality, transparency, electrical insulation, low moisture absorption, easy dyeing and low price, and has been widely used in electronics, automobiles, construction, Toys, packaging and other industries. However, polystyrene is easy to burn and drips heavily when burning. These shortcomings limit its popularization and use in occasions with high fire protection requirements. At present, the flammability of polystyrene is usually solved by adding halogenated flame retardants or adding phosphorus-containing organic or inorganic compounds. However, thes...

Examples

Embodiment 1

[0026] In a 250ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) of phenyl phosphate dichloride and 80ml of tetrahydrofuran, stir in an ice bath at -5 to 5°C, and after 20 minutes, add 21.2 g (0.21 mol) of triethylamine, and slowly add a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of tetrahydrofuran dropwise within 2 hours under continuous stirring, and continue to react for 4 hours. Then, 7.32 g (0.1 mol) of diethylamine was dissolved in 80 ml of tetrahydrofuran, and slowly dropped into the above reaction system under the condition of ice bath at -5-5° C. under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the obtained light yellow transparent liquid is the product of the present invention. The yield was 80%.

[0027] The obtained product was analyzed ...

Embodiment 2

[0031] In a 250ml three-necked flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml methylene chloride, stir in an ice bath, and after 10 minutes, add 21.2g (0.21 mol) triethylamine, then slowly dropwise added a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of dichloromethane in 2 hours under continuous stirring, and continued to react for 4 hours. Then 7.32 g (0.1 mol) of diethylamine was dissolved in 60 ml of dichloromethane, and slowly dropped into the above reaction system under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the obtained light yellow transparent liquid is the product of the present invention. The yield was 85%.

[0032] The obtained product was analyzed by nuclear magnetic resonance spectrum. The peak position of th...

Embodiment 3

[0035] In a 250ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml tetrahydrofuran, stir in an ice bath, and after 10 minutes, add 21.2g (0.21mol) Triethylamine, and a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of tetrahydrofuran was slowly added dropwise within 2 hours under continuous stirring, and the reaction was continued for 4 hours. Then diethylamine was dissolved in 80ml of tetrahydrofuran, and slowly dropped into the above reaction system under continuous stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the obtained yellow transparent liquid is the product of the present invention. The yield was 80%.

[0036]The obtained product was analyzed by nuclear magnetic resonance spectrum. The peak position of the chemical shift ...

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