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Phosphorus-containing PTT fire-resistant copolyesters/ nano composite material and preparation method thereof

A technology of trimethylene phthalate and nano-composite material is applied in the field of phosphorus-containing polytrimethylene terephthalate flame retardant copolyester/nano-composite material and preparation thereof, and can solve the problems of affecting the mechanical properties of materials, being difficult to disperse uniformly, Flame retardancy decline and other problems, to achieve the effect of easy promotion, improved fiber performance, and low cost

Active Publication Date: 2010-05-19
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the added non-reactive flame retardant is dispersed in the matrix resin in a free form, it will not only greatly affect the mechanical properties of the material because it is difficult to disperse evenly, but also cause migration, frosting, etc. Lead to decreased flame retardancy or failure

Method used

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  • Phosphorus-containing PTT fire-resistant copolyesters/ nano composite material and preparation method thereof
  • Phosphorus-containing PTT fire-resistant copolyesters/ nano composite material and preparation method thereof
  • Phosphorus-containing PTT fire-resistant copolyesters/ nano composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] First, 16.22 g of montmorillonite was modified according to the method described in CN 1396206A.

[0032] First add 291g of dimethyl terephthalate, 286g of 1,3-propanediol and 0.31g of zinc acetate catalyst into the reaction vessel and stir to raise the temperature. Until methanol is produced, then add 3.12g of DDP to the system, continue to stir and react at 170-200°C until no more water is produced. Add 0.12 g of tetrabutyl titanate catalyst and the above-prepared modified montmorillonite to the system, vacuumize the system until the system pressure is 400 Pa, and raise the temperature to 190-220 ° C for 1 hour for pre-condensation. Then evacuate until the system pressure is ≤50Pa, and at the same time raise the reaction temperature to 250-270°C for 3 hours for polycondensation.

Embodiment 2

[0034] First add 291g of dimethyl terephthalate, 346g of 1,3-propanediol, and 0.16g of zinc acetate catalyst into the reaction vessel and stir to raise the temperature. Until methanol is produced, then add 16.36g of DDP to the system, continue to stir and react at 190-210°C until no more water is produced. Add 0.26g of tetrabutyl titanate catalyst and 0.348g of nano-silicon dioxide pre-dispersed in 5ml of 1,3-propanediol to the system, and evacuate the system to a pressure of 200Pa, and raise the temperature to 190-220°C for 1 hour of precondensation. Then evacuate until the system pressure is ≤100Pa, and at the same time raise the reaction temperature to 220-250°C for polycondensation for 5 hours. The resulting product was pulverized and solid-state polymerized at a temperature of 160° C. for 0.5 hours.

Embodiment 3

[0036]First add 291g of dimethyl terephthalate, 236g of 1,3-propanediol, and 0.17g of cobalt acetate catalyst into the reaction vessel and stir to raise the temperature. Until methanol is produced, then add 34.78g of DDP to the system, continue to stir and react at 160-180°C until no more water is produced. Add 0.12g of tetrabutyl titanate catalyst and 6.68g of mecca stone to the system, and evacuate the system until the pressure of the system is 200Pa, and keep the temperature at 190-210°C for 0.3 hours for pre-condensation. Then evacuate until the system pressure is ≤100Pa, and at the same time raise the reaction temperature to 220-250°C for 0.5 hours of polycondensation.

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Abstract

The invention discloses a phosphorus-containing PTT fire-resistant copolyesters / nano composite material which is formed after carrying out in-situ polymerization on terephthalic acid or dimethyl terephthalate, 1,3-propanediol, a phosphorus-containing fire-resistant monomer and inorganic nano-particles, wherein the phosphorus-containing fire-resistant monomer accounts for 1-20 percent of the fire-resistant copolyesters in weight, the inorganic nano-particles account for 0.1-15 percent of the fire-resistant copolyesters in weight, and the intrinsic viscosity of the composite material is 0.5-2.0dL / g. The invention also discloses a preparation method thereof. Because the phosphorus-containing fire-resistant monomer is a reactive flame retardant and the nano-particles are added in an in-situ composite way, the composite material has enhanced fire resistance and mechanical property and obtains higher molecular weight by further solid phase polymerization. The invention has simple technical operation, low cost and easy application.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing poly(trimethylene terephthalate) flame-retardant composite material and its preparation, and specifically relates to a phosphorus-containing poly(trimethylene terephthalate) flame-retardant copolyester / nano-composite material and a preparation method thereof. Background technique [0002] Polytrimethylene terephthalate (PTT) is an aromatic polyester synthesized from terephthalic acid (PTA) and 1,3-propanediol (PDO) through esterification and polycondensation (and solid-state polycondensation). Since industrialized production in the 1990s, it has been widely used in various fields of people's daily activities. They can be made into fibers, films, engineering plastics, etc. In particular, because PTT fiber not only has the chemical resistance and stain resistance of PET fiber, but also has the softness of nylon and the bulkiness of acrylic fiber, its elastic recovery and recovery rate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08K9/00C08K3/34C08G63/692C08G63/80
Inventor 陈洪兵王玉忠张怡陈力汪秀丽王德义
Owner SICHUAN UNIV
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