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High-temperature self-crosslinking flame-retardant, smoke-suppressing, and anti-droplet copolyester based on benzamide structure and its preparation method and application

A self-crosslinking and anti-droplet technology, which is applied in the direction of additive processing, can solve the problems of not being able to be used as textile fiber raw materials, the large amount of smoke released by flame-retardant polyester, and the damage to the processing performance of polyester, so as to inhibit the organic small Molecular volatilization, excellent flame retardancy, and the effect of promoting char formation

Active Publication Date: 2020-08-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most phosphorus-containing flame-retardant polyesters achieve flame retardancy by taking away heat through molten droplets, which is the flame-retardant mechanism of "promoting molten droplets"; molten droplets will cause secondary damage, which is a modern flame-retardant that needs to be avoided. of
On the other hand, many flame-retardant polyesters release a large amount of smoke when burning, which is not good for escape in the event of a fire.
[0004] In order to solve the contradiction between flame retardancy and anti-dripping, ZL 201010124613.8 added anti-dripping agents such as polytetrafluoroethylene and its derivatives, inorganic fillers and glass fibers to the polyester base material, although it improved the performance of the composite material. Drop resistance, but it also destroys the excellent processing performance of polyester itself, so that it cannot be used as a raw material for textile fibers
In addition, although ZL201110043163.4 discloses the self-crosslinking of phenylacetylene groups at high temperature to achieve flame retardancy and anti-droplet of polyester, in this patent, the introduction of phenylacetylene structural units will cause the smoke release of copolyester The amount is larger than that of ordinary polyester; secondly, in order to obtain a copolyester with better flame retardancy and anti-melt drop effect, it is necessary to introduce a higher molar ratio of monomer

Method used

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  • High-temperature self-crosslinking flame-retardant, smoke-suppressing, and anti-droplet copolyester based on benzamide structure and its preparation method and application
  • High-temperature self-crosslinking flame-retardant, smoke-suppressing, and anti-droplet copolyester based on benzamide structure and its preparation method and application
  • High-temperature self-crosslinking flame-retardant, smoke-suppressing, and anti-droplet copolyester based on benzamide structure and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Add 582g dimethyl terephthalate, 310g ethylene glycol, 46.9g dimethyl 5-benzamido-1,3-phthalate, 1.0g zinc acetate and 0.8g antimony trioxide to the reaction kettle During the process, fill the reactor with nitrogen to remove the air in the kettle; carry out the reaction at 180°C for 2 hours at normal pressure, raise the temperature to 200°C for 2 hours, and then raise the temperature to 220°C for 1 hour, and the transesterification reaction is completed; then conduct the polycondensation reaction at 220-240°C in a low vacuum 0.5~1.5h, then polycondensation reaction at 230~250°C for 1~3 hours under high vacuum (pressure<60Pa), discharge and water cooling.

[0055] The intrinsic viscosity [η] of the high-temperature self-crosslinking flame-retardant, smoke-suppressing and anti-melting droplet copolyester copolyester is 0.75dL / g; the oxygen index is 27.3%, the vertical combustion level is V-2, and the cone calorimetry test The peak heat release rate p-HRR is 664kW / m 2 , ...

Embodiment 2

[0057] Add 582g dimethyl terephthalate, 310g ethylene glycol, 93.9g dimethyl 5-benzamido-1,3-phthalate, 1.0g zinc acetate and 0.8g antimony trioxide to the reaction kettle Among them, after carrying out transesterification reaction and polycondensation according to the step and the condition that embodiment 1 provides, discharging.

[0058] The intrinsic viscosity [η] of the high-temperature self-crosslinking flame-retardant, smoke-suppressing and anti-droplet copolyester copolyester is 0.70dL / g; the oxygen index is 28.7%, the vertical combustion level is V-2, and the cone calorimetry test The peak heat release rate p-HRR is 573kW / m 2 , the total smoke emission is 1201m 2 / m 2 .

Embodiment 3

[0060] Add 582g dimethyl terephthalate, 310g ethylene glycol, 140.9g dimethyl 5-benzamido-1,3-phthalate, 1.0g zinc acetate and 0.8g antimony trioxide to the reaction kettle Among them, after carrying out transesterification reaction and polycondensation according to the step and the condition that embodiment 1 provides, discharging.

[0061] The intrinsic viscosity [η] of the high-temperature self-crosslinking flame-retardant, smoke-suppressing and anti-melting droplet copolyester copolyester is 0.64dL / g; the oxygen index is 29.8%, the vertical combustion level is V-1, and the cone calorimetry test The peak heat release rate p-HRR is 398kW / m 2 , the total smoke emission is 994m 2 / m 2 .

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Abstract

The invention discloses a high-temperature self-crosslinked flame retardant smoke suppressing molten drop-resistant copolyester based on a benzamide structure. The polyester is composed of structuralunits as shown in I, II and III or structural units as shown in I, II and IV through irregular copolymerization. The intrinsic viscosity [Aita] of the copolyester is 0.10-1.40 dL / g, the limit oxygen index is 21.0-40.0%, the vertical combustion grade is V-2-V-0 grade. The peak heat release rate p-HRR in a cone calorimetric test is reduced by 10-80% compared with that of pure PET, and the total smoke release amount is reduced by 5-70% compared with that of pure PET. The invention also discloses a preparation method thereof. By introducing a high-temperature crosslinked group as a benzamide groupor a benzamide phenylacetylene group, the corresponding copolyester is free of crosslinking action in processing and polymerizing processes, so that the thermoplastic workability of polyester is retained. Meanwhile, as a result of a tackifying effect and a high char forming property caused by self-crosslinking action at high temperature or combustion, the copolyester has excellent flame-retarding, smoke-suppressing and molten drop-resisting effects.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant, smoke-suppressing and anti-droplet copolyester and its preparation. Specifically, the high-temperature self-crosslinking flame-retardant smoke-suppressing anti-melt droplet copolyester based on benzamide structure and its preparation method and application relate to a class of high-temperature self-crosslinking flame-retardant and smoke-suppressing copolyesters containing benzamide structure. Copolyester with drop resistance and its preparation method and application. Background technique [0002] Semi-aromatic polyesters, such as polyethylene terephthalate (PET) and polytrimethylene terephthalate (PTT), are widely used as packaging barrier materials due to their excellent performance and low price, Synthetic fibers, films and engineering plastics. However, the inherent flammability of polyester materials limits its further application. In addition, when polyester is burned, a large amo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685C08G63/86
CPCB33Y70/00C08G63/6856C08G63/866
Inventor 王玉忠陈琳倪延朋付腾吴志正汪秀丽
Owner SICHUAN UNIV
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