Benzene imide structure based high-temperature self-crosslinking copolyester with effects of flame retardancy, smoke suppression and melt drop resistance and preparation method of copolyester

A benzimide and benzimide-containing technology, which is applied in the field of copolyester and its preparation, can solve the problems of thermal stability damage of polyester, achieve good thermal stability, excellent flame retardancy, and inhibit small organic molecules Volatile effect

Active Publication Date: 2018-08-03
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the presence of 2-hydroxyethyl hypophosphorous acid will promote the decomposition of polyester substrates, damage the thermal stability of polyester, and limit the application of materials in some fields.

Method used

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  • Benzene imide structure based high-temperature self-crosslinking copolyester with effects of flame retardancy, smoke suppression and melt drop resistance and preparation method of copolyester
  • Benzene imide structure based high-temperature self-crosslinking copolyester with effects of flame retardancy, smoke suppression and melt drop resistance and preparation method of copolyester
  • Benzene imide structure based high-temperature self-crosslinking copolyester with effects of flame retardancy, smoke suppression and melt drop resistance and preparation method of copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 582g (3mol) of dimethyl terephthalate, 310g (5mol) of ethylene glycol, 53g (0.15mol) of N-(2-methylphenyl)-4,5-dimethoxybenzimide, Add 1.0g of zinc acetate and 0.8g of antimony trioxide into the reaction kettle, fill with nitrogen to remove the air in the kettle; carry out the reaction at 180°C for 2 hours under normal pressure, heat up to 200°C for 2h, then raise the temperature to 220°C for 1h, the ester The exchange reaction is completed; then the polycondensation reaction is carried out at 220-240° C. for 0.5-1.5 hours in low vacuum, and then the polycondensation reaction is carried out at 230-250° C. for 1-3 hours under high vacuum (pressure < 60 Pa), and the material is discharged and water-cooled.

[0049] The intrinsic viscosity [η] of the copolyester is 1.12dL / g; the oxygen index is 24.2%, the vertical combustion level is V-2, and the peak heat release rate p-HRR in the cone calorimetry test is 658kW / m 2 , the total smoke emission is 1713m 2 / m 2 .

Embodiment 2

[0051] 582g (3mol) of dimethyl terephthalate, 310g (5mol) of ethylene glycol, 106g (0.3mol) of N-(2-methylphenyl)-4,5-dimethoxybenzimide, 1.0 g of zinc acetate and 0.8 g of antimony trioxide were added to the reaction kettle, and after transesterification and polycondensation were carried out according to the steps and conditions given in Example 1, the materials were discharged.

[0052] The intrinsic viscosity [η] of the copolyester is 1.01dL / g; the oxygen index is 26.3%, the vertical combustion level is V-2, and the peak heat release rate p-HRR in the cone calorimetry test is 531kW / m 2 , the total smoke emission is 1584m 2 / m 2 .

Embodiment 3

[0054] 582g (3mol) of dimethyl terephthalate, 310g (5mol) of ethylene glycol, 159g (0.45mol) of N-(2-methylphenyl)-4,5-dimethylcarboxylate benzimide, 1.0 g of zinc acetate and 0.8 g of antimony trioxide were added to the reaction kettle, and after transesterification and polycondensation were carried out according to the steps and conditions given in Example 1, the materials were discharged.

[0055] The intrinsic viscosity [η] of the copolyester is 1.05dL / g; the oxygen index is 28.0%, the vertical combustion level is V-1, and the peak heat release rate p-HRR in the cone calorimetry test is 462kW / m 2 , the total smoke emission is 1426m 2 / m 2 .

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Abstract

The invention discloses a benzene imide structure based high-temperature self-crosslinking copolyester with effects of flame retardancy, smoke suppression and melt drop resistance. Copolyester is prepared from structural units represented by I, II and III or structural units represented by I, II and IV through random copolymerization, wherein the characteristic viscosity [eta] of copolyester is 0.41-1.12 dL / g, and the limit oxygen index is 24.2%-38.7%; the vertical combustion class is in a range from V-2 to V-0; the p-HRR (peak of heat release rate) in a cone calorimetry test is reduced by 7.1%-72.1% as compared with that of pure PET, and total smoke release is decreased by 2.0%-59.2% as compared with that of pure PET. The invention further discloses a preparation method of copolyester. Ahigh-temperature self-crosslinking group introduced in the preparation process is a benzene imide group, and prepared copolyeste cannot be subjected to crosslinking during processing and polymerization, so that thermoplastic processability of polyester is retained; meanwhile, due to the tackifying effect and high charring property brought by the self-crosslinking action at high temperature or during combustion, prepared copolyester has excellent flame retardancy, smoke suppression and melt drop resistance effects.

Description

technical field [0001] The invention belongs to the technical field of copolyester and its preparation. It specifically relates to a kind of copolyester containing benzimide structure with high temperature self-crosslinking flame retardancy, smoke suppression and droplet resistance and a preparation method thereof. Background technique [0002] Semi-aromatic polyester, especially polyethylene terephthalate (PET), has become the most widely used synthetic fiber due to its excellent physical and chemical properties, and is widely used in various fields in daily life. However, the polyester material itself is extremely flammable and does not self-extinguish after being ignited, which severely limits its application in some fields that require flame retardancy. In addition, polyester will produce molten dripping during the burning process, which will threaten people's life safety and may cause "secondary fire"; in the burning process, it is usually accompanied by a large amount...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/685C08G63/78
CPCC08G63/6856C08G63/78
Inventor 王玉忠刘博文陈力郭德明刘晓锋龙家伟罗曦丁晓敏史小慧
Owner SICHUAN UNIV
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