Preparation method of modified ammonium polyphosphate-black phosphorus flame-retardant PET polyester

A technology of ammonium polyphosphate and black phosphorus, which is applied in the field of flame retardant engineering plastics, can solve the problems of unstable surface state and poor stability of nano black phosphorus, and achieve the effects of high stability, high thermal stability and reducing the amount of addition.

Active Publication Date: 2020-07-10
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the surface state of nano black phosphorus is unstable, so the stability is poor when used as a flame retardant

Method used

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  • Preparation method of modified ammonium polyphosphate-black phosphorus flame-retardant PET polyester
  • Preparation method of modified ammonium polyphosphate-black phosphorus flame-retardant PET polyester

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[0034] A preparation method of modified ammonium polyphosphate-black phosphorus flame-retardant PET polyester, comprising the following steps:

[0035] 1) Preparation of composite flame retardant: Add the ground 1-2μm black phosphorus to the DMF solution at a solid-to-liquid ratio of 1.5-2.5g / L, and ultrasonically treat it at 0°C-5°C for 2-6h to obtain black phosphorus nanoparticles Dispersion of flakes, suction filtration and drying to obtain black phosphorus nano flakes; dissolve phenolic resin and black phosphorus in absolute ethanol, ultrasonic 10-30mi; then add ammonium polyphosphate and dimethyl silicone oil, stir at room temperature for 1-3h, Filter the obtained mixture, wash with ethanol, and dry in vacuum for 8h-12h to obtain modified ammonium polyphosphate-black phosphorus nanosheet powder, that is, a composite flame retardant. The mass ratio of the phenolic resin, black phosphorus, absolute ethanol, ammonium polyphosphate and dimethyl silicone oil is 2-5:0.3-0.6:50-...

Embodiment 1

[0044] 1) Grinding 1.0 g of massive black phosphorus to 1-2 μm, adding it to 500 mL of DMF solution, and ultrasonically treating it at 0° C. for 4 hours to obtain a dispersion of black phosphorus nanosheets, and drying by suction to obtain black phosphorus nanosheets;

[0045] 2) Dissolve 3 g of phenolic resin and 0.5 g of black phosphorus nanosheets in 60 g of absolute ethanol, and sonicate for 20 min. Then 5 g of ammonium polyphosphate and 0.2 g of simethicone were added, stirred at room temperature for 2 h, the mixture was filtered, washed with ethanol, and dried in vacuum for 12 h to obtain modified ammonium polyphosphate-black phosphorus nanosheet powder.

[0046] 3) Put 80% of the total amount of ethylene glycol and all the terephthalic acid into the beating tank to make a mixed slurry, and the molar ratio of the total amount of ethylene glycol to terephthalic acid is 1.5:1;

[0047] 4) Put 15% ethylene glycol and a catalyst into a catalyst preparation kettle, stir evenly ...

Embodiment 2

[0054] 1) Grinding 1.0 g of massive black phosphorus to 1-2 μm, adding it to 500 mL of DMF solution, and ultrasonically treating it at 0° C. for 4 hours to obtain a dispersion of black phosphorus nanosheets, and drying by suction to obtain black phosphorus nanosheets;

[0055] 2) Dissolve 3 g of phenolic resin and 0.5 g of black phosphorus nanosheets in 60 g of absolute ethanol, and sonicate for 20 min. Then 5 g of ammonium polyphosphate and 0.2 g of simethicone were added, stirred at room temperature for 2 h, the mixture was filtered, washed with ethanol, and dried in vacuum for 12 h to obtain modified ammonium polyphosphate-black phosphorus nanosheet powder.

[0056] 3) Put 80% of the total amount of ethylene glycol and all the terephthalic acid into the beating tank to make a mixed slurry, and the molar ratio of the total amount of ethylene glycol to terephthalic acid is 1.5:1;

[0057] 4) Put 15% ethylene glycol and a catalyst into a catalyst preparation kettle, stir evenl...

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Abstract

The invention relates to the technical field of flame-retardant engineering plastics, and discloses a preparation method of modified ammonium polyphosphate-black phosphorus flame-retardant PET polyester, and the method comprises the following steps: 1) taking black phosphorus, ammonium polyphosphate, phenolic resin and simethicone as raw materials to prepare a composite flame retardant; 2) preparing mixed slurry from ethylene glycol and terephthalic acid; 3) preparing ethylene glycol and a catalyst into a catalyst solution; 4) mixing the composite flame retardant with ethylene glycol to prepare an additive suspension; 5) performing primary esterification; 6) performing secondary esterification; 7) performing pre-polycondensation; and 8) carrying out final polycondensation, cooling, discharging and dicing. The composite flame retardant is synthesized through a polymerization reaction, the stability of black phosphorus nanosheets and the compatibility of the black phosphorus nanosheets with a polymer matrix are improved by taking phenolic resin as the matrix, the flame-retardant stability is further improved through compounding of P and N flame-retardant auxiliaries, and the flame-retardant PET polyester material is high in flame-retardant efficiency and has excellent mechanical and high-temperature-resistant properties.

Description

technical field [0001] The invention relates to the technical field of flame-retardant engineering plastics, in particular to a method for preparing a modified ammonium polyphosphate-black phosphorus flame-retardant PET polyester. Background technique [0002] Polyethylene terephthalate (PET) is a widely used polymer resin, which has the advantages of excellent mechanical properties, physical properties, thermal properties and excellent dimensional stability. In some specific application fields, there is a requirement for flame retardant properties of PET, and ordinary PET composite materials cannot meet the requirements. [0003] Although traditional halogen-based flame retardants can bring good flame-retardant properties to materials, they will produce a lot of smoke and toxic and corrosive hydrogen halide gases during the combustion process, which does not meet the requirements of environmentally friendly development. Metal hydroxides are non-volatile and do not produce ...

Claims

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Application Information

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IPC IPC(8): C08L67/02C08L61/06C08L83/04C08K13/06C08K9/10C08K3/32C08K3/02C08G63/183
CPCC08L67/02C08G63/183C08K2201/011C08K2003/323C08K2003/026C08L2201/02C08L61/06C08L83/04C08K13/06C08K9/10C08K3/32C08K3/02
Inventor 胥荣威胡舒龙李院院产文涛郝莱丹
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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