Flame-retardant anti-dripping copolyester based on high-temperature self-crosslinking as well as preparation method and application of flame-retardant anti-dripping copolyester

A technology of self-crosslinking and copolyester, which is applied in the manufacture of fire-resistant and flame-retardant filaments, single-component polyester artificial filaments, etc., can solve the problem of destroying the mechanical properties and spinnability of polyester, but cannot solve the problem of polyester smoke release , environmental pollution and health issues, to achieve the effect of suppressing the generation of molten droplets, excellent flame retardant and anti-droplet performance, and suppressing volatilization

Active Publication Date: 2021-12-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Some of the currently published research results are mainly through the addition of anti-droplet agents, such as polytetrafluoroethylene and its derivatives, glass fibers, silica, etc., to polyester, although these additives can improve the flame retardancy of polyester to a certain extent and anti-droplet effect, but in addition to greatly destroying the mechanical properties and spinnability of polyester, it cannot solve the problem of serious smoke release when polyester is burned. These additives will also be separated from polyester and released to the environment during use. Among them, there is the problem that the flame retardant effect is not durable, and long-term use will also bring potential environmental pollution and health problems

Method used

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  • Flame-retardant anti-dripping copolyester based on high-temperature self-crosslinking as well as preparation method and application of flame-retardant anti-dripping copolyester
  • Flame-retardant anti-dripping copolyester based on high-temperature self-crosslinking as well as preparation method and application of flame-retardant anti-dripping copolyester
  • Flame-retardant anti-dripping copolyester based on high-temperature self-crosslinking as well as preparation method and application of flame-retardant anti-dripping copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 498.0 g of terephthalic acid, 220.0 g of ethylene glycol, 7.98 g of 4-(phenylethynyl) phthalic acid, 36.6 g of 2,8-(2-hydroxyethoxy) potassium phenanthrene oxaphosphinate, Add 0.3g of antimony trioxide into the reaction kettle, fill with nitrogen to remove the air in the kettle, pressurize to 0.1MPa, raise the temperature to 240°C within 2 hours to start the esterification reaction, control the pressure in the kettle to 0.3-0.4MPa, and maintain 2 After ~4 hours, the pressure begins to drop to normal pressure, and the esterification reaction ends; then, the polycondensation reaction is carried out at 240°C for 0.5 to 2 hours in a low vacuum, and then the temperature is raised to 250~270°C, and the polycondensation reaction is carried out in a high vacuum (pressure<80Pa) for 1~2 hours. After 4 hours, the material was discharged and water-cooled.

[0054] The intrinsic viscosity [η] of the copolyester is 0.85dL / g; the limiting oxygen index is 27.0%; the vertical combustion...

Embodiment 2

[0056] 582.0g dimethyl terephthalate, 400.0g ethylene glycol, 159.6g 4-(phenylethynyl) phthalic acid, 25.2g (3-(2-hydroxyethoxy)-3-oxopropane Base) (phenyl) sodium phosphinate, 0.2g manganese acetate and 0.25g germanium dioxide were added to the reaction kettle, filled with nitrogen to remove the air in the kettle body; the reaction was carried out at 180-220°C under normal pressure for 2-6 hours, and the transesterification The reaction is completed; then polycondensation is carried out at 240-250° C. for 0.5-2 hours in low vacuum, and then at 250-270° C. for 1-4 hours under high vacuum (pressure < 80 Pa). The material is discharged and water-cooled.

[0057] The intrinsic viscosity [η] of the copolyester is 0.62dL / g; the limiting oxygen index is 30.5%; the vertical combustion rating is V-2; the peak heat release rate p-HRR in the cone calorimetry test is 312kW / m 2 , the total smoke release TSR is 801 m 2 / m 2 .

Embodiment 3

[0059] 388.0g dimethyl terephthalate, 194g dimethyl isophthalate, 400.0g ethylene glycol, 79.8g 4-(phenylethynyl) phthalic acid, 52.5g (3,5-bis(formyl Oxycarbonyl) phenyl) potassium phosphonate, 40.2g isophthalic acid-5-sodium sulfonate, 0.28g isopropyl titanate were added to the reaction kettle, and after esterification and polycondensation were carried out according to the steps and conditions of Example 2 ,Discharge.

[0060]The intrinsic viscosity [η] of the copolyester is 0.90dL / g; the limiting oxygen index is 31.0%; the vertical combustion rating is V-0, and no droplet is produced in the test; the p-HRR in the cone calorimetry test is 222kW / m 2 , TSR is 640m 2 / m 2 .

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Abstract

The flame-retardant anti-dripping copolyester based on high-temperature self-crosslinking disclosed by the invention is composed of structural units represented by I, II, III and IV, the intrinsic viscosity [eta] of the copolyester is 0.20-3.50 dL / g, the limit oxygen index is 23.0-60.0%, and the vertical burning grade is V-2 to V-0 grade. The invention also discloses a preparation method and application of the flame-retardant anti-dripping copolyester. Due to the introduced high-temperature self-crosslinking group and ionic group, the melt viscosity and the melt strength of the copolyester during combustion are improved, and meanwhile, the charring capacity of the copolyester is effectively enhanced, so that the copolyester disclosed by the invention shows excellent flame retardance and molten drop resistance. The preparation process of the copolyester is mature, simple and convenient to operate, easy to control and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of flame retardant and anti-melt droplet copolyester and its preparation and application. Specifically, the invention relates to a class of copolyester with high temperature self-crosslinking property, flame retardancy and anti-melt droplet property and its preparation methods and applications. Under the combined effect of high-temperature self-crosslinking flame-retardant monomers and ionic monomers, this type of copolyester not only improves its melt viscosity and melt strength through chemical crosslinking and physical crosslinking at high temperature, but also greatly It enhances its char-forming ability during combustion, and thus exhibits excellent flame-retardant and anti-droplet performance. Background technique [0002] Semi-aromatic polyester (referred to as polyester), such as polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), etc., because of their excellent thermal stability...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/688C08G63/685C08G63/78D01F6/92D01F1/07
CPCC08G63/6928C08G63/6886C08G63/6856C08G63/6888C08G63/6858C08G63/78D01F6/92D01F1/07
Inventor 王玉忠陈琳倪延朋付腾吴万寿刘博文赵海波汪秀丽
Owner SICHUAN UNIV
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