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Copolyester crosslinking monomer, copolyester based on monomer and preparation method thereof

A technology of cross-linking monomers and copolyesters, applied in the direction of organic chemistry, etc., can solve the problems of undiscovered copolyester glass ring transition temperature, limited combustion effect, complex synthesis, etc., to achieve high glass transition temperature and low cost , The effect of simple synthesis process

Active Publication Date: 2015-04-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in general, these chemical structures are not only complicated to synthesize and expensive; more importantly, the combustion effect is limited when the low content of polyester is added without destroying the properties of polyester itself.
In addition, judging from the current research results, there is no way to find a cheap, olefin-containing cyclic flame-retardant monomer that can greatly increase the ring transition temperature of copolyester glass

Method used

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  • Copolyester crosslinking monomer, copolyester based on monomer and preparation method thereof
  • Copolyester crosslinking monomer, copolyester based on monomer and preparation method thereof
  • Copolyester crosslinking monomer, copolyester based on monomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 55.3g dimethyl terephthalate, 40.9g ethylene glycol, 5.3g 5-(norbornene-2,3-dicarboxyimino)-1,3-dimethylisophthalate (DMTMI ), 0.061g of zinc acetate and 0.061g of tetrabutyl titanate were added to the polymerization bottle, filled with nitrogen to remove the air in the polymerization bottle; within 2 hours, the temperature was raised to 180°C to start the esterification reaction, and at the same time, nitrogen was kept flowing for 3 After 1.5 hours, the temperature was gradually raised to 200°C, 220°C, and 240°C, and the esterification reaction was completed; thereafter, the polycondensation reaction was carried out at 240-260°C in low vacuum (400Pa~100Pa) for 0.5 hours, and then the temperature was raised to 260°C ℃~270℃ high vacuum (pressure <60Pa) polycondensation reaction for 1~3 hours, the target product can be obtained. In the resulting product, DMTMI accounted for 5% by mole of the dibasic acid structure.

[0052] The intrinsic viscosity [η] of the polyester is...

Embodiment 2

[0054] 52.5g dimethyl terephthalate, 40.9g ethylene glycol, 10.7g 5-(norbornene-2,3-dicarboxyimino)-1,3-dimethylisophthalate (DMTMI ), 0.062g of zinc acetate and 0.062g of tetrabutyl titanate were added into the polymerization bottle, and the target product was obtained after esterification reaction and polycondensation were carried out according to the steps and conditions given in Example 1. In the resulting product, DMTMI accounted for 10% of the mole percent of the dibasic acid structure.

[0055] The intrinsic viscosity [η] of the polyester is 0.62 dL / g; the oxygen index is 27.7%, the glass transition temperature is 89.5°C, and the peak heat release rate p-HRR in the cone calorimetry test is 525 kW / m 2 .

Embodiment 3

[0057] 46.7g dimethyl terephthalate, 40.9g ethylene glycol, 21.4g 5-(norbornene-2,3-dicarboxyimino)-1,3-dimethylisophthalate (DMTMI ), 0.064g of zinc acetate and 0.052g of tetrabutyl titanate were added into the polymerization bottle, and the target product was obtained after esterification reaction and polycondensation were carried out according to the steps and conditions given in Example 1. In the resulting product, DMTMI accounted for 20% of the mole percent of the dibasic acid structure.

[0058] The intrinsic viscosity [η] of the polyester is 0.60 dL / g; the oxygen index is 26.0%, the glass transition temperature is 98.6°C, and the peak heat release rate p-HRR in the cone calorimetry test is 268kW / m 2 .

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Abstract

The invention discloses a copolyester crosslinking monomer, a copolyester based on the monomer and a preparation method thereof. The copolyester is prepared by carrying out random copolymerization on structural units disclosed as I, II and III. The intrinsic viscosity number [eta] of the copolyester is 0.20-0.94 dL / g. The invention also discloses a preparation method of the copolyester. The introduced crosslinking group is a cyclic olefin structure which has a unique structure and can be subjected to chemical decomposition rearrangement with double bond at high temperature, causing crosslinking, thereby greatly enhancing the complex viscosity of the copolyester in the combustion process; and thus, the carbonization capacity is enhanced, so the copolyester has excellent flame retardancy and molten drop resistance, and the glass transition temperature of the copolyester can be obviously enhanced. The structure is simple to synthesize and low in cost; and the structure is free of the volatilizable halogen, phosphorus and other toxic substance elements in the traditional flame retardant, and thus, belongs to a green flame-retardant copolyester.

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 new type of flame-retardant anti-droplet copolyester and its preparation method. Background technique [0002] Polyester (here mainly refers to dimethyl terephthalate, PET) is widely used in fiber, packaging materials, electronic appliances, medical and health, construction and other fields due to its excellent comprehensive performance. After decades of development in my country, it has become The world's number one polyester producer. However, the glass transition temperature of polyester itself is only 76.5°C, and it has serious flammability and droplet characteristics, which greatly limit its application prospects in other fields. [0003] Judging from the current research status, for polyester materials, the flame retardants currently used in mass production are still halogen-conta...

Claims

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Application Information

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IPC IPC(8): C07D209/48C07D209/76C07D491/08C07D207/452C08G63/685C08G63/85C08G63/83
Inventor 王玉忠董雪陈力段荣涛
Owner SICHUAN UNIV
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