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Phosphorus heterocycle inflaming retarding copolyester ionomer and preparation method thereof

A copolyester and ionomer technology, applied in the manufacture of fire-resistant and flame-retardant filaments, single-component copolyester artificial filaments, etc., can solve the problems of poor hydrophilicity and dyeability, lack of flame-retardant properties, and fabric costs Higher problems, to achieve the effect of increasing melt viscosity, excellent flame retardancy and anti-dripping, excellent anti-dripping

Active Publication Date: 2013-02-13
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] As we all know, in addition to the problems of flammability and melt dripping, polyester fiber also has the shortcomings of poor hydrophilicity and dyeability. The dyeing conditions not only make the fabric cost high and the chromatogram is narrow, but also the large amount of organic solvents used in the dyeing process will cause serious environmental pollution, and the introduction of anionic groups into the molecular chain can improve the dyeability of polyester fibers
In 1958, the dyeable copolyester (CDP) ionomer fiber developed by Dupont had good affinity for cationic dyes, and ECDP, which was further modified on the basis of CDP, realized the cationic effect of polyester under normal pressure. Dye boiling, but none of the above ionomers have flame retardant properties

Method used

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  • Phosphorus heterocycle inflaming retarding copolyester ionomer and preparation method thereof
  • Phosphorus heterocycle inflaming retarding copolyester ionomer and preparation method thereof
  • Phosphorus heterocycle inflaming retarding copolyester ionomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] First add 415g of terephthalic acid (TPA), 217mL of ethylene glycol (EG) and 0.23g of tetrabutyl titanate into the reaction kettle, fill with nitrogen to remove the air in the kettle, then pressurize to 0.1MPa, and gradually raise the temperature to 240°C , start esterification, and control the pressure in the kettle to 0.3-0.4MPa. After 1 hour of esterification, the temperature gradually rises to 260°C. When the esterification reaction ends when anhydrous is generated, the pressure drops to normal pressure; Inject nitrogen, slowly add 1.10g of ethylene glycol solution of phosphorus-containing flame retardant ionic monomer 2,8-(2-hydroxyethoxy) carbonylphenanthrene oxaphosphinate (SDHPPO) into the reaction kettle, and control the temperature When the temperature is above 220°C, stop the nitrogen flow after the addition, and start vacuuming. The system is pre-condensed at 260°C for 0.5h in low vacuum, and then enters the high vacuum stage (<100Pa), polycondensates at 280°...

Embodiment 2

[0060] Firstly, 415g of terephthalic acid (TPA), 217mL of ethylene glycol (EG) and 0.23g of tetrabutyl titanate were added to the reaction kettle, and the esterification reaction was carried out according to the method in Example 1. After the esterification, the pressure drop To normal pressure, nitrogen gas is slowly introduced into the reactor, and the ethylene glycol of 10.75g of phosphorus-containing flame-retardant ionic monomer 2,8-(2-hydroxyethoxy)sodium carbonylphenanthreneoxaphosphinate (SDHPPO) The solution was slowly added to the reactor, and then the polycondensation was carried out according to the method of Example 1.

[0061] The intrinsic viscosity [η] of the phosphorus-containing heterocyclic flame-retardant copolyester ionomer is 0.89dL / g, the limiting oxygen index LOI is 25.0, and the peak heat release rate is 442kW / m 2 .

Embodiment 3

[0063] Firstly, 415g of terephthalic acid (TPA), 217mL of ethylene glycol (EG) and 0.23g of tetrabutyl titanate were added to the reaction kettle, and the esterification reaction was carried out according to the method in Example 1. After the esterification, the pressure drop To normal pressure, nitrogen gas is slowly introduced into the reactor, and the ethylene glycol of 32.25g of phosphorus-containing flame-retardant ionic monomer 2,8-(2-hydroxyethoxy)sodium carbonylphenanthreneoxaphosphinate (SDHPPO) The solution was slowly added to the reactor, and then the polycondensation was carried out according to the method of Example 1.

[0064]The intrinsic viscosity [η] of the phosphorus-containing heterocyclic flame-retardant copolyester ionomer is 0.73dL / g, the limiting oxygen index LOI is 25.5, and the peak heat release rate is 367kW / m 2 .

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Abstract

The invention discloses a phosphorus heterocycle inflaming retarding copolyester ionomer which is formed by introducing structure units represented by III and IV on the basis of polyester structure units represented by I and II and conducting random copolymerization. The intrinsic viscosity [eta]of the phosphorus heterocycle inflaming retarding copolyester ionomer is 0.2-1.1 dL / g. A preparation method of the ionomer is further disclosed. Due to the fact that phosphorus ion groups are introduced, inflaming retarding modification and ionization modification can be simultaneously achieved without adding other fire retardants, carbon formation effect and stable 'physical cross-linking' effect produced by 'iron aggregate' of the phosphorus ion groups improve melt viscosity of high polyester, and simultaneously the polyester has excellent inflaming retarding and molten drop resistance. The ionomer can directly serve as raw materials for preparing fibers, engineering plastics, film and the like.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing flame-retardant copolyester ionomer and its preparation. Specifically, the invention relates to a novel phosphorus-containing heterocyclic flame-retardant copolyester ionomer and a preparation method thereof. The ionized flame-retardant modified polyester of the present invention can not only endow the polyester fiber with dyeing performance, but also endow the polyester with excellent flame-retardant and anti-droplet performance. Background technique [0002] In recent years, fires have become more and more frequent, and the losses caused by fires have become increasingly serious. The occurrence of fires will not only cause property losses, but also easily lead to heavy casualties. With the development of science and technology and the improvement of people's living standards, people pay more and more attention to the prevention and control of fire. [0003] Polyester fiber is a s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692D01F6/84D01F1/07
Inventor 王玉忠张怡陈力何明昕赵晶晶倪延朋翟筠秋
Owner SICHUAN UNIV
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