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Flame retardant anti-droplet copolyester based on benzimidazole structure, and preparation method thereof

A technology of benzimidazole and copolyester, which is applied in the field of flame-retardant and droplet-resistant copolyester and its preparation, can solve the problems of high cost, shortened polyester processing window, limited effect, etc., and achieves the improvement of glass transition temperature, Excellent anti-dripping, excellent flame retardant effect

Active Publication Date: 2018-08-14
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chemical crosslinking method will shorten the processing window of polyester to a certain extent, while the physical crosslinking method of ionic agglomeration has limited effect on improving the melt viscosity, and the cost of the above monomers is relatively high

Method used

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  • Flame retardant anti-droplet copolyester based on benzimidazole structure, and preparation method thereof
  • Flame retardant anti-droplet copolyester based on benzimidazole structure, and preparation method thereof
  • Flame retardant anti-droplet copolyester based on benzimidazole structure, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 415g of terephthalic acid, 220mL of ethylene glycol, 14.1g of 2-(4-carboxyphenyl)-1H-benzimidazole-5-carboxylic acid and 0.212g of tetrabutyl titanate into the reaction kettle, and fill with nitrogen Exclude the air in the kettle body, 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 will be reduced to normal pressure, and the esterification reaction is over; thereafter, the low vacuum polycondensation reaction is carried out at 260-270℃ for 0.5h, and then the temperature is raised to 270℃ high vacuum (pressure<60Pa) polycondensation reaction is carried out for 1~3h, and the material is discharged. Water cooling is enough.

[0049] The intrinsic viscosity [η] of the copolyester is 1.36dL / g; the glass transition temperature i...

Embodiment 2

[0051] Add 415g of terephthalic acid, 220mL of ethylene glycol, 35.25g of 2-(4-carboxyphenyl)-1H-benzimidazole-5-carboxylic acid and 0.212g of tetrabutyl titanate into the reactor, and follow the implementation After the steps and conditions given in example 1 carried out esterification and polycondensation reaction, discharging.

[0052] The intrinsic viscosity [η] of the copolyester is 1.29dL / g; the glass transition temperature is 92°C, the limiting oxygen index is 28.0%, the vertical burning level is V-2 level, and the melting dripping phenomenon is obviously improved, twice Flame droplets are produced and ignite the absorbent cotton during ignition. There are only a few droplets during the test, and the sample can self-extinguish; but the peak heat release rate p-HRR in the cone calorimetry test is 465kW / m 2 , the total flue gas generation is 14.5m 2 .

Embodiment 3

[0054] Add 415g of terephthalic acid, 235mL of ethylene glycol, 70.5g of 2-(4-carboxyphenyl)-1H-benzimidazole-5-carboxylic acid and 0.212g of tetrabutyl titanate into the reactor, and follow the implementation After the steps and conditions given in example 1 carried out esterification and polycondensation reaction, discharging.

[0055] The intrinsic viscosity [η] of the copolyester is 1.26dL / g; the glass transition temperature is 96°C, the limiting oxygen index is 31.0%, the vertical combustion rating is V-2, and the melting dripping phenomenon is significantly improved, the first There is no droplet in the first ignition, and only one flaming droplet is produced in the second ignition, and the absorbent cotton is ignited; the peak heat release rate p-HRR in the cone calorimetry test is 355kW / m 2 , the total flue gas generation is 11.2m 2 .

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Abstract

The invention discloses a flame retardant anti-droplet copolyester based on a benzimidazole structure, and a preparation method thereof. The copolyester is composed of structural units represented byformula I, II, III or I, II and IV, the characteristic viscosity [eta] of the copolyester is 0.48-1.36 dL / g, and the limit oxygen index is 25.0-42.0%; the glass transition temperature of the copolyester is 7-62 DEG C higher than that of pure PET; the vertical burning grade is V-2 to V-0 grade; the peak heat release rate p-HRR in cone calorimetry test is 42.8-82.5% lower than that of the pure PET;and the total smoke release amount is 15.8-69.0% lower than that of the pure PET. The benzimidazole structure introduced in the invention can rapidly form a large amount of charcoal during combustionin order to achieve excellent flame retarding, droplet resisting and smoke suppressing effects, can maintain the original processing window of the polyester and realize multi-time repeated processing,and also can greatly improve the glass transition temperature of the copolyester; and the preparation method has the advantages of mature process, simplicity and convenience in operation, and high easiness in industrial production.

Description

technical field [0001] The invention belongs to the technical field of flame retardant and anti-melt droplet copolyester and its preparation. Specifically, the invention relates to high glass transition temperature, high char forming, flame retardant and anti-melt droplet copolymerization containing benzimidazole structure Esters and methods for their preparation. Background technique [0002] Semi-aromatic polyesters, such as polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), for their good heat resistance, dimensional stability, and chemical resistance It is widely used in the fields of packaging materials, synthetic fibers, films and engineering plastics because of its advantages such as non-toxicity and recyclability. However, the glass transition temperature of polyester itself is not high (such as the glass transition temperature of PET is only 76 ° C), and has serious flammability and easy melt dripping disadvantages, which greatly limit its appli...

Claims

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Application Information

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IPC IPC(8): C08G63/685
CPCC08G63/6856
Inventor 王玉忠倪延朋吴万寿陈琳汪秀丽秦子皓李启天
Owner SICHUAN UNIV
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