High-temperature self-crosslinking flame-retardant anti-dripping copolyester and preparation method thereof

A self-crosslinking and copolyester technology, which is used in the field of flame retardant and anti-droplet copolyester and its preparation, high temperature self-crosslinking, can solve problems such as limiting the application scope of polyester, and achieve excellent resistance. The effect of burning and anti-droplet, good solvent resistance and good char formation

Active Publication Date: 2011-09-07
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the addition of these substances can achieve a certain anti-melt drop effect, it also greatly limits the application range of polyester, especially it cannot be used as a raw material for spinning fibers. This is undoubtedly the same as polyester is mostly used as raw materials for spinning fibers. Contradictory purpose

Method used

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  • High-temperature self-crosslinking flame-retardant anti-dripping copolyester and preparation method thereof
  • High-temperature self-crosslinking flame-retardant anti-dripping copolyester and preparation method thereof
  • High-temperature self-crosslinking flame-retardant anti-dripping copolyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 860g of terephthalic acid, 433mL of ethylene glycol and 0.301g of antimony trioxide into the reaction kettle, fill with nitrogen to remove the air in the kettle, pressurize to 0.1MPa; raise the temperature to 240°C within 2h to start the esterification reaction, control the kettle The internal pressure is 0.3-0.4MPa. After maintaining for 2 hours, the pressure begins to decrease. After 1.5 hours, the temperature gradually rises to 260°C, the pressure drops to normal pressure, and the esterification reaction ends; nitrogen is slowly introduced into the reactor, and 6.89g The ethylene glycol solution of the cross-linking monomer 2-phenylacetylene terephthalic acid is added to the reaction kettle, and the temperature is controlled above 210°C. When the system temperature rises slowly to 260°C, the nitrogen flow is stopped and the vacuum polymerization stage is entered. Firstly, conduct polycondensation reaction in low vacuum at 260-270°C for 0.5h, then raise the tempera...

Embodiment 2

[0044] Add 860g of terephthalic acid, 433mL of ethylene glycol, 13.78g of cross-linking monomer 4-phenylacetylene phthalic anhydride and 0.301g of antimony trioxide into the reactor, and perform esterification according to the steps and conditions given in Example 1 After reaction and polycondensation, discharge.

[0045] The intrinsic viscosity [η] of the polyester is 0.74dL / g; the oxygen index is 23.0%, the vertical combustion level is V-2, and the number of drops from two ignition to extinguishment in the vertical combustion is a total of 25 drops. In the cone calorimetry test The peak heat release rate p-HRR is 820kW / m 2 .

Embodiment 3

[0047] 860g of terephthalic acid, 433mL of ethylene glycol and 0.301g of antimony trioxide were added to the reactor, and the esterification reaction was carried out according to the steps and conditions given in Example 1; Nitrogen, and the crosslinking monomer 5-phenylacetylene-1 of 69.41g, the ethylene glycol solution of 3-isophthalate is added in the reaction kettle, after carrying out polycondensation according to the step and the condition that embodiment 1 provides again, out material.

[0048] The intrinsic viscosity [η] of the polyester is 0.85dL / g; the oxygen index is 25%, the vertical combustion level is V-2, and the number of drops from two ignition to extinguishment in the vertical combustion is a total of 10 drops. In the cone calorimetry test The peak heat release rate p-HRR is 596kW / m 2 .

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Abstract

The invention discloses a high-temperature self-crosslinking flame-retardant anti-dripping copolyester which is prepared by introducing a structural unit shown as IV in the specification or introducing structural units shown as III and IV in the specification by random copolymerization on the basis of structural units of synthetic polyester shown as I and II in the specification, and the intrinsic viscosity [eta] of the prepared high-temperature self-crosslinking copolyester is 0.25-1.25dL / g. The invention also discloses the preparation method of the high-temperature self-crosslinking copolyester. Because the crosslinking group introduced in the invention is a high-temperature self-crosslinking group, on the premise of not affecting the preparation and forming of the polyester, self-crosslinking can be realized at higher temperature, and the melt viscosity of the polyester is improved through the char formation effect and stable chemical crosslinking of the self-crosslinking group, thereby performing combined action with the phosphorus-containing flame-retardant structural unit IV and endowing the polyester with better flame-retardant and anti-dripping properties.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant and droplet-resistant copolyester and its preparation. Specifically, the present invention relates to a class of copolyesters with high-temperature self-crosslinking properties, flame retardancy and anti-dropping properties and a preparation method thereof. Due to the joint action of flame retardant monomers and crosslinking monomers, this type of copolyester increases the melt viscosity of polyester through chemical crosslinking at high temperature, thus endowing polyester with better flame retardant and droplet resistance properties. Background technique [0002] Polyester, especially polyethylene terephthalate (PET), occupies a large share in synthetic fibers because of its high modulus, high strength, high elasticity, shape retention and heat resistance. In recent years, in addition to being used as fiber materials, it has also been widely used in packaging, construction, automobiles,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692
Inventor 王玉忠赵海波杨君驰刘博文葛欣国陈力
Owner SICHUAN UNIV
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