Droplet-resistant flame-retardant polyester, nanometer compound material thereof and method for preparing same

Abstract

The invention discloses droplet-resistant flame-retardant polyester. The flame-retardant polyester is prepared by random copolymerization of a branched monomer, terephthalic acid or dimethyl terephthalate, ethylene glycol and flame-retardant monomer, wherein the branched monomer is an aliphatic compound or aromatic compound having three or more functional groups; and the flame-retardant monomers adopts any of the following structures. The invention also discloses a method for preparing the droplet-resistant flame-retardant polyester, a nanometer compound material containing the droplet-resistant flame-retardant polyester and a method for preparing the nanometer compound material. Because the droplet-resistant flame-retardant polyester provided by the invention simultaneously contains the branched monomer and the fire retardant having the droplet-resistant effect, the melt viscosity of the droplet-resistant flame-retardant polyester at the high temperature is greatly improved, the sensitivity of the droplet-resistant flame-retardant polyester to temperature is lowered, and the droplet-resistant effect is good; because of the nanometer effect and the blocking effect, the nanometer compound material shows better droplet-resistant effect; and the polyester and the nanometer compound material can be directly used as raw materials for preparing fibers, engineering plastics, films and the like.

Description

technical field

[0001] The invention belongs to the technical field of flame-retardant polyester and polyester nano composite material and its preparation. In particular, it relates to a copolyester having flame retardancy and droplet resistance, a nanocomposite material thereof and a preparation method thereof. Background technique

[0002] Polyester (here specifically refers to polyethylene terephthalate, PET) is one of the three synthetic polymer materials in synthetic fibers, because of its high modulus, high strength, high elasticity, shape retention and heat resistance The advantages of anti-corrosion and other advantages make it the largest and most widely used fiber variety in synthetic fibers in 1972. However, the oxygen index of polyester is only 21.0, which is a flammable fiber, which greatly restricts its use in occasions that have certain requirements for fire protection. Especially after the promulgation of the national standard (GB20286-2006) on the combusti...

Examples

Embodiment 1

[0039] 835g terephthalic acid, 425ml ethylene glycol, 0.5g branched monomer triethylene glycol trimesate, 30g flame retardant monomer DPA (9,10-dihydro-oxa-10 phosphophenanthrene -propionic acid) and 0.301g of antimony trioxide were added to the reaction kettle, first filled with nitrogen to remove the air in the kettle, then pressurized to 0.1Mpa, and raised the temperature to 240°C within 2h, and continued to raise the pressure to 0.3-0.4MPa, Esterification reaction for 2 hours; after maintaining the temperature and pressure for 1.5 hours, gradually increase the temperature to 260°C, and maintain the water outlet speed, and reduce the pressure to normal pressure after about 0.5 hours, and the esterification reaction ends. Thereafter, the polycondensation reaction was carried out at 260-270° C. for 0.5 h in low vacuum, and then the temperature was raised to 275-285° C., and the polycondensation reaction was carried out at high vacuum (pressure < 60 Pa) for 2 hours. Then, the m...

Embodiment 2

[0042] 769g terephthalic acid, 415ml ethylene glycol, 30g branched monomer triethylene glycol trimellitate, 60g flame retardant monomer DPA (9,10-dihydro-oxa-10 phosphorophenanthrene- Propionic acid) and 0.348g ethylene glycol antimony join in the reactor, after carrying out esterification and polycondensation reaction by the step that embodiment 1 provides, condition, discharging, water cooling gets final product.

[0043] The intrinsic viscosity [η] of the flame-retardant polyester was 0.86dL / g, the oxygen index was 35.4%, and the vertical combustion grade was V-0.

Embodiment 3

[0045] 589g terephthalic acid, 410ml ethylene glycol, 50g branched monomer triethylene glycol trimellitate, 150g flame retardant monomer DPP (9,10-dihydro-oxa-10 phosphorophenanthrene- Succinic acid) and 0.348g ethylene glycol antimony join in the reactor, after carrying out esterification and polycondensation reaction by the step that embodiment 1 provides, condition, discharging, water cooling gets final product.

[0046] The intrinsic viscosity [η] of the flame-retardant polyester was 1.02dL / g, the oxygen index was 36%, and the vertical combustion rating was V-0.

technical field

[0001] The invention belongs to the technical field of flame-retardant polyester and polyester nano composite material and its preparation. In particular, it relates to a copolyester having flame retardancy and droplet resistance, a nanocomposite material thereof and a preparation method thereof. Background technique

[0002] Polyester (here specifically refers to polyethylene terephthalate, PET) is one of the three synthetic polymer materials in synthetic fibers, because of its high modulus, high strength, high elasticity, shape retention and heat resistance The advantages of anti-corrosion and other advantages make it the largest and most widely used fiber variety in synthetic fibers in 1972. However, the oxygen index of polyester is only 21.0, which is a flammable fiber, which greatly restricts its use in occasions that have certain requirements for fire protection. Especially after the promulgation of the national standard (GB20286-2006) on the combusti...

Examples

Embodiment 1

[0039] 835g terephthalic acid, 425ml ethylene glycol, 0.5g branched monomer triethylene glycol trimesate, 30g flame retardant monomer DPA (9,10-dihydro-oxa-10 phosphophenanthrene -propionic acid) and 0.301g of antimony trioxide were added to the reaction kettle, first filled with nitrogen to remove the air in the kettle, then pressurized to 0.1Mpa, and raised the temperature to 240°C within 2h, and continued to raise the pressure to 0.3-0.4MPa, Esterification reaction for 2 hours; after maintaining the temperature and pressure for 1.5 hours, gradually increase the temperature to 260°C, and maintain the water outlet speed, and reduce the pressure to normal pressure after about 0.5 hours, and the esterification reaction ends. Thereafter, the polycondensation reaction was carried out at 260-270° C. for 0.5 h in low vacuum, and then the temperature was raised to 275-285° C., and the polycondensation reaction was carried out at high vacuum (pressure < 60 Pa) for 2 hours. Then, the m...

Embodiment 2

[0042] 769g terephthalic acid, 415ml ethylene glycol, 30g branched monomer triethylene glycol trimellitate, 60g flame retardant monomer DPA (9,10-dihydro-oxa-10 phosphorophenanthrene- Propionic acid) and 0.348g ethylene glycol antimony join in the reactor, after carrying out esterification and polycondensation reaction by the step that embodiment 1 provides, condition, discharging, water cooling gets final product.

[0043] The intrinsic viscosity [η] of the flame-retardant polyester was 0.86dL / g, the oxygen index was 35.4%, and the vertical combustion grade was V-0.

Embodiment 3

[0045] 589g terephthalic acid, 410ml ethylene glycol, 50g branched monomer triethylene glycol trimellitate, 150g flame retardant monomer DPP (9,10-dihydro-oxa-10 phosphorophenanthrene- Succinic acid) and 0.348g ethylene glycol antimony join in the reactor, after carrying out esterification and polycondensation reaction by the step that embodiment 1 provides, condition, discharging, water cooling gets final product.

[0046] The intrinsic viscosity [η] of the flame-retardant polyester was 1.02dL / g, the oxygen index was 36%, and the vertical combustion rating was V-0.

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