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Expanded-char-forming, flame-retardant and melt-dropping-resistant copolyester based on polyphenyl ether structure and preparation method of copolyester

A technology of copolyester and polyphenylene ether, which is applied in the field of flame-retardant and droplet-resistant copolyester and its preparation, can solve problems such as personal injury and property loss, and achieve secondary combustion, high char formation efficiency and rate, The effect of excellent flame retardancy and droplet resistance

Active Publication Date: 2015-06-17
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Severe droplets will not only cause "secondary combustion" and cause unnecessary property damage, but also very likely to cause serious injury to people in the fire scene
At present, the flame retardancy of traditional flame retardant polyester is usually achieved by promoting the degradation of polyester and accelerating the melting and dripping to take away the heat and ignition source. Therefore, there is a certain contradiction between flame retardancy and anti-melting dripping. How to solve and coordinate This contradiction has always been a difficult problem in polyester flame retardant research.

Method used

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  • Expanded-char-forming, flame-retardant and melt-dropping-resistant copolyester based on polyphenyl ether structure and preparation method of copolyester
  • Expanded-char-forming, flame-retardant and melt-dropping-resistant copolyester based on polyphenyl ether structure and preparation method of copolyester
  • Expanded-char-forming, flame-retardant and melt-dropping-resistant copolyester based on polyphenyl ether structure and preparation method of copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 860g of terephthalic acid, 419mL of ethylene glycol, 97.8g of 1,4-bis[4-(2-hydroxyethoxy)phenoxy]benzene and 0.344g of tetrabutyl titanate were added to the reaction kettle, and the Exclude the air in the kettle with nitrogen, 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, after maintaining for 2 hours, the pressure begins to decrease, and the temperature gradually rises to 260 after 1.5 hours ℃, the pressure drops to normal pressure, and the esterification reaction ends; thereafter, the polycondensation reaction is carried out at 260-270 ℃ for 0.5h in low vacuum, and then the temperature is raised to 270 ℃ for high vacuum (pressure <60Pa) polycondensation reaction for 1-3 hours, and the material is discharged , water-cooled.

[0041] The intrinsic viscosity [η] of the copolyester is 0.65dL / g; the limiting oxygen index is 26.0%; the vertical combustion grade is V...

Embodiment 2

[0043] 860g of terephthalic acid, 404mL of ethylene glycol, 195.7g of 1,4-bis(4-methyl carboxyphenoxy)benzene and 0.344g of tetrabutyl titanate were added to the reaction kettle, as given in Example 1. After esterification and polycondensation reaction according to the steps and conditions, the material is discharged.

[0044] The intrinsic viscosity [η] of the copolyester is 0.68dL / g; the limiting oxygen index is 28.0%; the vertical combustion grade is V-2 level, and the number of drops from two ignition to extinguishment in vertical combustion is 14 drops; The peak heat release rate p-HRR in the calorimetric test is 558kW / m 2 .

Embodiment 3

[0046] 860g of terephthalic acid, 404mL of ethylene glycol, 202.9g of 1,4-bis(4-methylcarboxyphenoxy)-2-methylbenzene and 0.344g of tetrabutyl titanate were added to the reaction kettle, After carrying out the esterification and polycondensation reaction according to the steps and conditions given in Example 1, the material is discharged.

[0047] The intrinsic viscosity [η] of the copolyester is 0.74dL / g; the limiting oxygen index is 28.5%; the vertical burning level is V-2 level, and the number of drops from two times of ignition to extinguishment in vertical burning is a total of 8 drops; The peak heat release rate p-HRR in the thermal test is 521kW / m 2 .

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Abstract

The invention discloses expanded-char-forming, flame-retardant and melt-dropping-resistant copolyester based on a polyphenyl ether structure. The copolyester is prepared by introducing a structure unit expressed as the formula III on the basis of synthetic polyester structure units expressed as the formulae I and II through a random copolymerization process. The intrinsic viscosity [eta] of the prepared expanded-char-forming, flame-retardant and melt-dropping-resistant copolyester is 0.43-0.95 dL / g; the extreme oxygen index is 25.5-34.5%; the vertical combustion grade is between V-2 and V-0; the peak heat release rate p-HRR in a cone heat test is 198-658 kW / m<2>. The invention further discloses a preparation method of the copolyester. According to the copolyester, the monomer containing the polyphenyl ether structure can be subject to a rearrangement reaction at high temperature to form a stable structure with a plurality of aromatic rings or a plurality of aromatic oxygen-containing heterocyclic rings, so that the copolyester is extremely high in expanded-char-forming rate and quality, and high in flame-retardant performance and melt-dropping-resistant performance. The preparation method of the copolyester is mature in process, simple and convenient to operate, and easy for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant and droplet-resistant copolyester and its preparation. Specifically, the invention relates to a kind of copolyester with high-temperature rearrangement, expansion into charcoal, flame-retardant and droplet-resistant copolyester and its preparation method. This type of copolyester adopts modified monomers based on polyphenylene ether structure. It does not require additional flame retardant monomers, but uses the free radicals generated by the polyphenylene ether structure at high temperatures to connect to each other and undergo rearrangement reactions. , The large aromatic ring structure formed to obtain an obvious swelling carbon layer, thus endowing the copolyester with excellent flame retardancy and droplet resistance. Background technique [0002] Polyethylene terephthalate (PET) is one of the thermoplastic synthetic polymer materials with the largest output today because of its good ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/85C08G63/86
Inventor 王玉忠郭德明付腾阮超张文强吴嘉宁王晓琳汪秀丽陈力
Owner SICHUAN UNIV
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