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Azobenzene structure based high-temperature self-cross-linked expanded flame-retardant anti-dripping copolyester and preparation method thereof

A technology of intumescent flame retardant and copolyester, which is applied in the field of flame retardant and anti-droplet copolyester and its preparation, can solve the problems of high raw material cost, limited application range of copolyester, clogging of spinneret, etc., and achieve good mechanical properties Performance, good heat insulation and oxygen insulation, good flame retardant and droplet resistance

Active Publication Date: 2013-01-09
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the addition of these substances greatly limits the application range of copolyester, especially these infusible materials block the spinneret because they do not melt during the copolyester melt spinning process, so that they can no longer be used as raw materials for textile fibers
In addition, ZL201110043163.4 discloses that phenylalkynes (phenylacetylene phthalic anhydride, etc.) The cost is high, and the cost can be reduced only after mass production

Method used

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  • Azobenzene structure based high-temperature self-cross-linked expanded flame-retardant anti-dripping copolyester and preparation method thereof
  • Azobenzene structure based high-temperature self-cross-linked expanded flame-retardant anti-dripping copolyester and preparation method thereof
  • Azobenzene structure based high-temperature self-cross-linked expanded flame-retardant anti-dripping copolyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Add 332g of terephthalic acid, 195g of ethylene glycol, 27g of 3,5-azophthalic acid and 0.144g of antimony trioxide into the reactor, fill with nitrogen to remove the air in the reactor, and then pressurize to 0.1MPa; Raise the temperature to 240°C within 2 hours to carry out the esterification reaction. Control the pressure in the kettle to 0.3-0.4 Mpa. After maintaining for 2 hours, the pressure begins to drop. Within 1.5 hours, the temperature gradually rises to 260°C, the pressure drops to normal pressure, and the esterification reaction ends. ;Condensation in low vacuum at 260°C for 1 hour, then heat up to 275°C in vacuum (pressure 2 .

Embodiment 2

[0058] 332g terephthalic acid, 205g ethylene glycol, 54g 3,5-azophthalic acid and 0.146g antimony trioxide were added to the reactor, and the esterification reaction was carried out according to the steps and conditions given in Example 1 and After polycondensation, discharge. The intrinsic viscosity of the copolyester is 0.78dL / g; the oxygen index is 27.0%, the vertical combustion level is V-2, and the number of drips from two ignition to extinguishment in vertical combustion is 2 times (the drips are not formed by the melt Droplets, which are solid carbon residues), the peak heat release rate pHRR in the cone calorimetry test is 500kW / m 2 .

Embodiment 3

[0060] 332g terephthalic acid, 223g ethylene glycol, 108g 3,5-azophthalic acid and 0.156g antimony trioxide were added to the reactor, and the esterification reaction was carried out according to the steps and conditions given in Example 1 and After polycondensation, discharge. The intrinsic viscosity of the copolyester is 0.86dL / g; the oxygen index is 30.0%, the vertical combustion level is V-0, there is no droplet from two ignition to extinguishment in the vertical combustion, and the peak heat release rate pHRR in the cone calorimetry test 400kW / m 2 .

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Abstract

The invention discloses azobenzene structure based high-temperature self-cross-linked expanded flame-retardant anti-dripping copolyester and a preparation method thereof. The copolyester is composed of structural units represented as I, II and III or structural units represented as I, II, III and IV by means of random copolymerization, and the intrinsic viscosity [eta] of the copolyester is 0.25-1.30dL / g. A high-temperature self-cross-linked group introduced into the copolyester is an azobenzene-structured compound with a unique pi-pi large conjugated system, has no influence on copolyester synthesis and processing and can be heated to burn for quick thermochemical crosslinking to form carbon at high temperature to form a separation layer, so that excellent flame retardation and anti-dripping effects can be obtained. The selected compound with the azobenzene structure is cheap, and the method is mature in process, 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 droplet-resistant copolyester and its preparation. Specifically, the invention relates to a class of copolyesters with high-temperature self-crosslinking, expansion flame retardancy and droplet resistance and a preparation method thereof. This type of copolyester can use crosslinking monomers containing azobenzene structure alone to increase the melt viscosity of the copolyester through chemical crosslinking at high temperature, and at the same time a small part of the uncrosslinked azobenzene structure can be released Nitrogen is released to expand the carbon layer on the surface of the material, thereby endowing the copolyester with intumescent flame retardant and anti-droplet properties; it is also possible to use phosphorus-containing flame-retardant monomers and cross-linking monomers containing azobenzene structures to act together, so that the copolyester The P-N synergistic effe...

Claims

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Application Information

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IPC IPC(8): C08G63/692C08G63/685
Inventor 王玉忠敬新柯郭德明张瑶翟飞玉汪秀丽陈力吴嘉宁黄维
Owner SICHUAN UNIV
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