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Phosphorus-containing flame-retardant polyester ionomer/nanocomposite material and preparation method thereof

A technology of nanocomposite materials and flame-retardant copolyesters, which is applied in the field of phosphorus-containing flame-retardant copolyester ionomer/nanocomposite materials and its preparation, can solve the problems of poor comprehensive properties of materials, and achieve improved crystallization properties and good The effect of flame retardancy

Active Publication Date: 2014-09-17
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a kind of phosphorus-containing flame-retardant copolyester ionomer / nanocomposite material for the problems existing in the prior art. The composite material has good flame retardancy, droplet resistance and crystallization performance. It can overcome the problem of poor overall performance of materials obtained by using phosphorus-containing reactive flame retardants alone

Method used

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  • Phosphorus-containing flame-retardant polyester ionomer/nanocomposite material and preparation method thereof
  • Phosphorus-containing flame-retardant polyester ionomer/nanocomposite material and preparation method thereof
  • Phosphorus-containing flame-retardant polyester ionomer/nanocomposite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0060] First add 830g of terephthalic acid, 434mL of ethylene glycol and 0.46g of tetrabutyl titanate into the reaction kettle, pressurize to 0.1MPa, stir and heat up to 240°C under nitrogen protection to start esterification, control the pressure to 0.3MPa, about 1h After that, raise the temperature to 260°C and continue the esterification until no water is produced, and the pressure drops to normal pressure. After vacuuming at 260°C for about 0.5h, the excess ethylene glycol is pumped out, and then the vacuum is stopped. Nitrogen is introduced into the system, and after returning to normal pressure Into the reaction kettle, add dropwise the ethylene glycol containing 44.6g phosphorus-containing ionic monomer 2,8-(2-hydroxyethoxy)carbonylphenanthreneoxaphosphinate potassium (DHPPO-K) at a rate of 2 to 3 drops / second. Alcohol solution and 20.38g of octadecyltrimethylammonium chloride modified montmorillonite pre-dispersed in 150ml of ethylene glycol, and control the system temp...

Embodiment 2

[0062] First, 830g of terephthalic acid, 434mL of ethylene glycol and 0.46g of tetrabutyl titanate were added to the reactor, and the esterification reaction was carried out according to the method of Example 1 (the difference was that the pressure was controlled at 0.4MPa). After the esterification was completed, , the pressure is reduced to normal pressure, vacuumize at 260°C for about 0.5h, stop the vacuum after pumping out excess ethylene glycol, feed nitrogen into the system, return to normal pressure, and inject it into the reaction kettle at a rate of 2 to 3 drops / second Add dropwise the ethylene glycol solution containing 66.9g phosphorus ion monomer 2,8-(2-hydroxyethoxy) carbonyl phenanthrene oxa hypophosphite potassium and 5.11g pre-dispersed octadecyl in 50ml ethylene glycol Trimethyl ammonium chloride modified montmorillonite, and the temperature of the system is controlled above 220° C. during the dropping process, and the polycondensation can be carried out accord...

Embodiment 3

[0064] First, 830g of terephthalic acid, 434mL of ethylene glycol, 0.46g of tetrabutyl titanate, and 66.9g of phosphorus-containing ionic monomer 2,8-(2-hydroxyethoxy)carbonylphenanthreneoxaphosphinate potassium Diol solution is added in the reactor, carry out esterification reaction by the method for embodiment 1, after esterification finishes, pressure drops to normal pressure, vacuumizes at 260 ℃ for about 0.5h and stops vacuumizing after taking out excess ethylene glycol, to Nitrogen was introduced into the system, and after returning to normal pressure, 10.28g of octadecyltrimethylammonium chloride modified in advance dispersed in 120ml of ethylene glycol was added dropwise at a rate of 2 to 3 drops / second. Montmorillonite, and control the temperature of the system during the dropping process to be above 220° C., and then carry out polycondensation according to the method of Example 1 after adding (the difference is that the high vacuum polycondensation time is 0.5 hours)....

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Abstract

The invention discloses a phosphorus-containing flame-retardant polyester ionomer / nanocomposite material and a preparation method thereof. The phosphorus-containing flame-retardant polyester ionomer / nanocomposite material is prepared by in-situ polymerization of terephthalic acid or dimethyl terephthalate, ethylene glycol, phosphorus-containing ion monomers (i) or phosphorus-containing ion monomers (ii), inorganic nanoparticles or / and organic modified inorganic nanoparticles. The numbers of phosphorus-containing ion group structure units in the composite material account for 2% to 5% of the numbers of structure units of the terephthalic acid or the dimethyl terephthalate in the composite material. The content of the inorganic nanoparticles or / and organic modified inorganic nanoparticles accounts for 0.5 to 10% of the total mass of the composite material. Meanwhile, the phosphorus-containing flame-retardant polyester ionomer / nanocomposite material is excellent in flame retardance, melt drip resistance and crystallization resistance. The intrinsic viscosity of the phosphorus-containing flame-retardant polyester ionomer / nanocomposite material can reach 0.6dL / g to 1.0dL / g. Thus, the phosphorus-containing flame-retardant polyester ionomer / nanocomposite material can be directly taken as a raw material used for preparing fibers, engineering plastics, thin films and the like.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant nano-composite materials and their preparation, and in particular relates to a phosphorus-containing flame-retardant copolyester ionomer / nano-composite material and a preparation method thereof. Background technique [0002] Polyester (specifically polyethylene terephthalate, PET) is one of the most important semi-crystalline synthetic polymer materials because of its high strength, heat resistance, dimensional stability and chemical corrosion resistance, etc. Because of its advantages, it is widely used as packaging material, synthetic fiber, film and engineering plastic. Since the first commercialization of polyester in the 1950s, its application has developed rapidly. It can be seen in many fields such as clothing, decorative fabrics, food, electronic appliances, medical and health care, automobiles, and construction. At present, polyester fiber is one of the fastest growing, highest o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08K3/30C08K3/36C08K3/22C08K9/04C08K3/34C08K3/32C08K7/00C08K3/04C08L67/02
Inventor 王玉忠张怡倪延朋汪秀丽陈力何明昕王力
Owner SICHUAN UNIV
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