Heat-resistant flame-retardant polyester, polyester product, and preparation method and application thereof

A flame-retardant polyester and heat-resistant technology, used in polyester, heat-resistant and flame-retardant polyester, polyester products and their preparation fields, can solve problems such as insufficient heat resistance and flame retardant, and achieve high dependence and excellent resistance. Effects of thermal and flame retardancy

Active Publication Date: 2020-10-16
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The main purpose of the present invention is to provide a heat-resistant and flame-retardant polyester and its preparation method to overcome the shortcomings of existing FDCA-based polyesters with insufficient heat resistance and flame retardancy

Method used

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  • Heat-resistant flame-retardant polyester, polyester product, and preparation method and application thereof
  • Heat-resistant flame-retardant polyester, polyester product, and preparation method and application thereof
  • Heat-resistant flame-retardant polyester, polyester product, and preparation method and application thereof

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preparation example Construction

[0037] Another aspect of the embodiments of the present invention also provides a method for preparing heat-resistant and flame-retardant polyester, which includes:

[0038] Copolymerizing the first mixed reaction system comprising phosphorus-containing compound, dibasic acid and / or dibasic acid ester, dibasic alcohol, esterification and / or transesterification catalyst to obtain an intermediate product;

[0039] Making the second mixed reaction system comprising the intermediate product, polycondensation catalyst and stabilizer continue to react under vacuum conditions to obtain heat-resistant and flame-retardant polyester;

[0040] Wherein, the phosphorus-containing compound has a structure as shown in formula (I):

[0041]

[0042] Formula (I)

[0043] In formula (I), X and Y are independently selected from -OH, -OCOCH 3 or -O(CH 2 ) 2 OH,R 1 , R 2 , R 3 , R 4are independently selected from hydrogen, substituted or unsubstituted C1-C6 alkyl, substituted or unsubst...

Embodiment 1

[0117] Example 1 Dimethyl 2,5-furandicarboxylate, phosphorus-containing compound (formula (8)), ethylene glycol, and anhydrous zinc acetate were added to the reactor at a molar ratio of 1:0.3:2.0:0.001, nitrogen Under protective conditions, raise the temperature to 185°C, react for 3.5 hours, then add antimony trioxide with a molar weight of 1.0‰ of dimethyl 2,5-furandicarboxylate, and Triphenyl phosphate, the vacuum degree is 30Pa, the temperature is gradually raised to 245°C, and the reaction is carried out for 5.0 hours to obtain polyethylene-2,5-furandicarboxylate phosphorus-containing diol copolyester. The copolyester structure is shown in the following formula, 1 H-NMR (d-DMSO): δ=7.13ppm, furan ring, 2H; δ=4.55ppm, -CH 2 CH 2 -, 3.6H; δ=3.63ppm, methyl, 0.59H; δ=4.10-4.60ppm, CH, 0.1H; δ=6.41-7.72ppm, benzene ring, 1.4H. The glass transition temperature of the copolyester is 107°C, and the DSC spectrum is as follows figure 1 Shown; T in nitrogen 5% The thermal weigh...

Embodiment 2

[0120] Example 2 Dimethyl 2,5-furandicarboxylate, phosphorus-containing compound (formula (4)), ethylene glycol, and anhydrous zinc acetate were added to the reactor at a molar ratio of 1:0.05:2.1:0.0008, nitrogen Under protective conditions, raise the temperature to 190°C, react for 3 hours, then add antimony trioxide with a molar weight of 1.5‰ of dimethyl 2,5-furandicarboxylate, and phosphoric acid with a molar weight of 2,5-dimethyl furandicarboxylate of 2.0‰ Triphenyl ester, the vacuum degree is 60Pa, the temperature is gradually raised to 250°C, and the reaction is carried out for 4.0h to obtain the target product. through 1 H-NMR characterization revealed that the target product was polyethylene-2,5-furandicarboxylate phosphorus-containing diol copolyester, and its structural formula was shown in the following formula. The glass transition temperature of the copolyester is 91° C., and the flame retardancy test is V1 level.

[0121]

[0122] Wherein, m and n are int...

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Abstract

The invention discloses a heat-resistant flame-retardant polyester, a polyester product, and a preparation method and application thereof. The preparation method of the heat-resistant flame-retardantpolyester comprises the following steps: carrying out copolymerization reaction on a first mixed reaction system containing a phosphorus-containing compound, binary acid and / or binary acid ester, dihydric alcohol and an esterification and / or transesterification catalyst to obtain an intermediate product; and continuously reacting a second mixed reaction system containing the intermediate product,a polycondensation catalyst and a stabilizer under a vacuum condition to obtain the heat-resistant flame-retardant polyester. The phosphorus-containing compound has a structure as shown in the following formula, according to the invention, a phosphorus-containing compound is introduced into a synthesis system; the 2, 5-furandicarboxylic acid-based polyester has the advantages that the glass transition temperature and flame retardant property of the 2, 5-furandicarboxylic acid-based polyester can be effectively improved, so that the formed copolyester has excellent heat resistance and flame retardance, and can be widely applied to the fields of fire-fighting products, kitchen electrical products, food packaging, optics, building materials, decorative materials, automobile manufacturing, barrier films, barrier bottles, fibers, engineering plastics and the like.

Description

technical field [0001] The invention relates to a polyester, in particular to a heat-resistant and flame-retardant polyester, a polyester product and a preparation method and application thereof, belonging to the technical field of polymer materials. Background technique [0002] Polyethylene terephthalate (PET) is synthesized from terephthalic acid and ethylene glycol. It is widely used in chemical fiber, packaging materials, engineering plastics and other fields. The global annual output is more than 70 million tons, of which more than 40 million in China tons, and 80% is used for fiber manufacturing. At present, terephthalic acid (TPA), the main raw material for PET production, is completely dependent on the petrochemical product paraxylene (PX). Finding green manufacturing of PX and its derivatives has become an important proposition to maintain the sustainable development of the polyester industry. Bio-based polymer materials use sustainable biomass and its platform co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/78C08J5/18C08L67/02B32B33/00B32B27/36B32B27/18B32B27/06B32B7/10
CPCB32B7/10B32B27/06B32B27/18B32B27/36B32B33/00B32B2250/02B32B2307/306B32B2307/3065B32B2437/00C08G63/6926C08G63/78C08J5/18C08J2367/02
Inventor 刘小青王静刚费璇
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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