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Copolyester containing aromatic secondary amine structure and its preparation method and application

A technology of aromatic secondary amines and copolyesters, which is applied in the field of copolyesters containing aromatic secondary amine structures and its preparation and application, can solve the problems of destroying polyester mechanical properties and spinnability, and achieve good organic smoke volatilization , Improve the mechanical strength, smoke suppression and anti-droplet effect

Active Publication Date: 2022-06-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional flame retardant methods are difficult to achieve the "flame retardant", "anti-melt drop" and "smoke suppression" requirements of polyester at the same time, and to a certain extent will destroy the mechanical properties and spinnability of polyester

Method used

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  • Copolyester containing aromatic secondary amine structure and its preparation method and application
  • Copolyester containing aromatic secondary amine structure and its preparation method and application
  • Copolyester containing aromatic secondary amine structure and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 582.0 g of dimethyl terephthalate, 400.0 g of ethylene glycol, 47.0 g of 5-anilinocarbonyl-1,3-isophthalic acid dimethyl ester, 0.2 g of zinc acetate and 0.3 g of antimony trioxide were added to the In the reaction kettle, nitrogen is charged to remove the air in the kettle; the reaction is carried out under normal pressure at 180-220°C for 2-6 hours, and the transesterification reaction is completed; after that, the low-vacuum polycondensation reaction is carried out at 220-240°C for 0.5-1.5h, and then the reaction is carried out under high vacuum for 0.5-1.5 hours. (pressure<80Pa) at 250~270℃ for 1~4 hours of polycondensation reaction, discharging and water cooling.

[0047] The intrinsic viscosity [η] of the copolyester is 0.95dL / g; the limiting oxygen index is 25.0%; the vertical combustion grade is V-2, and there are droplets in the test, but the droplet phenomenon is obviously improved; The peak heat release rate p-HRR in thermal test is 608kW / m 2 , the total smo...

Embodiment 2

[0049] 582.0g of dimethyl terephthalate, 400.0g of ethylene glycol, 140.9g of 5-phenylaminocarbonyl-1,3-dimethyl isophthalate, 0.25g of isopropyl titanate were added to the reactor, After carrying out the transesterification and polycondensation reaction according to the steps and conditions given in Example 1, the material is discharged.

[0050] The intrinsic viscosity [η] of the copolyester is 0.80dL / g; the limiting oxygen index is 30.2%; the vertical combustion grade is V-0, and no droplets are produced in the test; the peak heat release rate in the cone calorimetry test p-HRR is 340kW / m 2 , the total smoke emission TSR is 954m 2 / m 2 ; The tensile strength is 90.6MPa.

Embodiment 3

[0052] 498.0g of terephthalic acid, 250.0g of ethylene glycol, 68.7g of 3,5-dihydroxy-N-phenylbenzamide, 0.3g of germanium dioxide were added to the reaction kettle, and nitrogen was charged to remove the air in the kettle. Pressurize to 0.1MPa, heat up to 220~240℃ to start the esterification reaction, control the pressure in the kettle to be 0.3~0.4MPa, after maintaining for 2~4h, gradually reduce the pressure to normal pressure, and the esterification reaction ends; after that, gradually heat up To 250°C, polycondensate in low vacuum for 0.5-1.5h, then perform polycondensation at 250-270°C for 1-4h in high vacuum (pressure < 80Pa), then discharge and cool with water.

[0053] The intrinsic viscosity [η] of the copolyester is 1.20dL / g; the limiting oxygen index is 28.0%; the vertical combustion grade is V-2, and there are droplets in the test, but the droplet phenomenon is obviously improved; Peak heat release rate p-HRR in thermal test is 575kW / m 2 , the total smoke emissio...

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Abstract

The copolyester containing aromatic secondary amine structure and its preparation method and application disclosed by the present invention, the copolyester is composed of structural units represented by I, II and III, and its intrinsic viscosity [η] is 0.30-3.5dL / g; the limiting oxygen index is 23.0-55.0%; the vertical combustion rating is V-2-V-0; the tensile strength is 5-300% higher than that of pure PET. The viscosity-increasing effect and char-forming effect of the flame-retardant unit containing aromatic secondary amine structure introduced in the present invention make the copolyester not only have excellent flame-retardant and anti-droplet performance, but also have good smoke suppression performance, which can It can be used alone in the fields of fibers, non-woven fabrics, engineering plastics, film materials, container materials, self-healing materials, shape memory materials or 3D printing materials, or as an additive for the modification of polymer materials.

Description

technical field [0001] The invention belongs to the technical field of copolyester containing aromatic secondary amine structure and its preparation and application. Specifically, the invention relates to copolyester containing aromatic secondary amine structure with flame retardancy, anti-dropping property and smoke suppression. and preparation method and application thereof. Background technique [0002] Semi-aromatic polyester (hereinafter referred to as polyester) is a class of linear polymers with rigid aromatic rings, flexible methylene and polar ester groups in the main chain, such as polyethylene terephthalate (PET) and polyethylene terephthalate. Butylene terephthalate (PBT), etc., are widely used in synthetic fibers, bottled materials and engineering plastics. But polyester is an extremely flammable polymer, which not only releases a lot of heat and smoke when burning, but is also accompanied by severe droplet behavior. As a class of widely used polymer material...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685C08G63/78C08G63/692C08G63/688
CPCC08G63/6856C08G63/78C08G63/6926C08G63/6886C08G2280/00
Inventor 王玉忠陈琳付腾倪延朋吴万寿段平慧汪秀丽
Owner SICHUAN UNIV
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