Phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer and preparation method thereof

A nylon elastomer, intrinsic flame retardant technology

Active Publication Date: 2019-08-30
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But unfortunately, so far, there have been no reports of intrinsically flame-retardant nylon elastomers.

Method used

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  • Phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer and preparation method thereof
  • Phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer and preparation method thereof
  • Phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Add 30g of caprolactam, 2.35g of adipic acid and 1.2ml of water together into a polymerization container, raise the temperature to 240°C for 4 hours under the protection of nitrogen, and carry out the ring-opening polycondensation of caprolactam, and then remove the water in the later stage of the reaction to obtain carboxyl-terminated Nylon prepolymer.

[0054] Add 13.69g of polyethylene glycol (Mn=1000), 0.78g of DOPO-HQ and 0.14g of catalyst tetrabutyl titanate to the above polymerization vessel, raise the temperature to 240°C for 2h under the protection of nitrogen, then raise the temperature to 260°C for 1h , and finally raised the temperature to 280°C and slowly vacuumed to 100Pa to react for 2h. The obtained product was extracted with boiling water for 8 hours, and the water was changed every hour; then the product was pre-dried in a blast oven, and finally dried in a vacuum oven at 80°C for 12 hours.

[0055] The limiting oxygen index LOI of the phosphorus-cont...

Embodiment 2

[0057] 30g of caprolactam, 2.35g of adipic acid and 1.2ml of water were added together into a polymerization container, and the ring-opening polycondensation of caprolactam was carried out according to the method of Example 1 to prepare a carboxy-terminated nylon prepolymer.

[0058] Add 12.88g of polyethylene glycol (Mn=1000), 1.04g of DOPO-HQ and 0.13g of catalyst tetrabutyl titanate into the above polymerization container, carry out esterification polycondensation and post-treatment according to the method of Example 1.

[0059] The limiting oxygen index LOI of the phosphorus-containing intrinsically flame-retardant thermoplastic nylon elastomer is 30.0, can pass the UL-94 vertical burning V-0 level, and the elongation at break and tensile strength can reach 608% and 32.37MPa respectively.

Embodiment 3

[0061] 30g of caprolactam, 2.35g of adipic acid and 1.2ml of water were added together into a polymerization container, and the ring-opening polycondensation of caprolactam was carried out according to the method of Example 1 to prepare a carboxy-terminated nylon prepolymer.

[0062] Add 12.08g of polyethylene glycol (Mn=1000), 1.31g of DOPO-HQ and 0.12g of catalyst tetrabutyl titanate into the above polymerization container, carry out esterification polycondensation and post-treatment according to the method of Example 1.

[0063] The limiting oxygen index LOI of the phosphorus-containing intrinsically flame-retardant thermoplastic nylon elastomer is 32.5, can pass the UL-94 vertical burning V-0 level, and the elongation at break and tensile strength can reach 468% and 27.33 MPa respectively.

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Abstract

The invention discloses a phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer and a preparation method thereof. The phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer is a nylon elastomer represented by the following structural general formula [I] obtained by the melt copolymerization reaction of a carboxyl-terminated nylon pre-polymer, a hydroxyl-terminated polyether polyol and a phosphorus-containing diol monomer, or is a nylon elastomer represented by the following structural general formula [II] obtained by the melt copolymerization reaction of a carboxyl-terminated phosphorus-containing nylon pre-polymer and a hydroxyl-terminated polyether polyol. The nylon elastomer is a multi-block copolymer, a phosphorus-containing reactive flameretardant is copolymerized and embedded in the molecular chain of the thermoplastic nylon elastomer, the effective flame retardancy at a low content can be realized, the durability is good, no migration problem exists, the ratio of a soft segment, a hard segment and the flame retardant can be adjusted, and demands of different mechanical properties of different application fields are satisfied under the premise of high efficiency flame retardant. The preparation method is simple, the raw materials are easily available, and the expanding production is favorable.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polymer elastomers and their preparation, in particular to a phosphorus-containing intrinsic flame-retardant thermoplastic nylon elastomer and a preparation method thereof, in particular to a phosphorus-containing reactive flame retardant copolymer embedded thermoplastic nylon elastic A polymer material with a bulk molecular chain and a preparation method thereof. Background technique [0002] Thermoplastic Nylon Elastomer (Thermoplastic Polyamide Elastomer, TPAE) is a typical block copolymer with polyamide as the hard segment and polyether or polyester as the soft segment. Among them, the hard segment mainly includes PA6, PA11 and PA12, and determines the hardness, melting point, relative density, tensile strength, resistance to various organic chemicals and other characteristics of the elastomer; the soft segment often uses PEG, PPG, PTMG or PCL, etc. , giving the material low temperatu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/44
CPCC08G69/44
Inventor 王玉忠卢鹏赵泽永李映明徐博仁邓聪赵盼盼何霜
Owner SICHUAN UNIV
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