Preparation method of halogen-free flame retardant nylon 66 polymer

A technology of flame retardant nylon and polymer, which is applied in the field of preparation of flame retardant nylon 66 to achieve the effect of high flame retardant decomposition temperature

Active Publication Date: 2014-12-17
LIAONING YINZHU CHEMTEX GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And use this polymer to spin to prepare a new type of flame-retardant nylon 66 fiber

Method used

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  • Preparation method of halogen-free flame retardant nylon 66 polymer
  • Preparation method of halogen-free flame retardant nylon 66 polymer
  • Preparation method of halogen-free flame retardant nylon 66 polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] DDP (DOPO derivative I) is selected as the reactive flame retardant in this example. The DDP Chinese alias [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphine -6-yl)methyl]succinic acid, its molecular structure is shown in formula (e), physical and chemical properties: molecular weight: 346.27; appearance: white powder; effective content: ≥98.5%; melting point: 191-192°C; flash Point: 303.5°C; Boiling point: 578.3°C; Density: 1.48g / cm 3 .

[0030]

[0031] The process of this embodiment is as follows:

[0032] 75 grams of flame retardant DDP and 25 grams of hexamethylenediamine are neutralized in aqueous solution at room temperature to form a salt solution. 1.5 kg of nylon 66 salt and 50°C desalted water are prepared to form a 50% nylon 66 salt solution. The two salt solutions were added to a stainless steel high-temperature autoclave. After the "three pumping and three charging" of high-purity nitrogen and vacuum, the temperature and pressure are raised to 220 ° C and 20 k...

Embodiment 2

[0034] The selected flame retardant is the same as in Example 1. The process of this embodiment is: 75 grams of flame retardant DDP and 25 grams of hexamethylenediamine are neutralized in an aqueous solution at room temperature to form a salt solution. 1.5 kg of nylon 66 salt, 30 g of caprolactam and desalted water at 50°C were prepared to form a 50% nylon 66 salt solution. The two salt solutions were added to a stainless steel high-temperature autoclave. After the "three pumping and three charging" of high-purity nitrogen and vacuum, the temperature and pressure are raised to 220 ° C and 20 kg, and kept for 2 hours; then start to exhaust steam and slowly reduce the pressure, and after about 30 minutes, it drops to atmospheric pressure and starts to heat up at the same time to 275-285°C. Keep the temperature at 275-285°C, evacuate to -0.09MPa, and keep it for 30 minutes. Nitrogen is used to break the vacuum, and the material is discharged and pelletized. A flame-retardant n...

Embodiment 3

[0036] DOPO-MDA (DOPO derivative II) is selected as the reactive flame retardant in this example, and the molecular structure of DOPO-MDA is shown in formula (f). Its effective content is ≥98.5%; melting point: 250-253°C. Molecular Structure:

[0037]

[0038] The process of this embodiment is as follows:

[0039]90 grams of flame retardant DOPO-MDA and 31.5 grams of adipic acid are neutralized in aqueous solution at room temperature to form a salt solution. 1.5 kg of nylon 66 salt and 50°C desalted water are prepared to form a 50% nylon 66 salt solution. The two salt solutions were added to a stainless steel high-temperature autoclave. After the "three pumping and three charging" of high-purity nitrogen and vacuum, the temperature and pressure are raised to 220 ° C and 20 kg, and kept for 2 hours; then the steam is exhausted and the pressure is lowered slowly, and the pressure is lowered to atmospheric pressure after about 30 minutes, and the temperature starts to rise...

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Abstract

The invention discloses a preparation method of a halogen-free flame retardant nylon 66 polymer and belongs to the field of a preparation technology of flame retardant nylon 66. According to the method, a copolymerization reaction between a reactive flame retardant-a DOPO derivative and diacid or diamine is firstly carried out to generate salt; and a copolymerization reaction between the generated salt and nylon 66 salt is then carried out so as to obtain the halogen-free flame retardant nylon 66 polymer. By selecting the new reactive flame retardant (the DOPO derivative) and through a matched polymerization formula and technology, the flame retardant nylon 66 polymer is developed. The flame retardant nylon 66 polymer has characteristics of high melting point, high decomposition temperature of the flame retardant, high molecular weight flame retardant polymer and high-strength flame resistant fibre, and fills gaps at home and abroad.

Description

technical field [0001] The invention relates to the technical field of preparation of flame-retardant nylon 66, in particular to a preparation method of a halogen-free flame-retardant nylon 66 polymer. Background technique [0002] The flame retardancy of nylon 66 is usually improved by blending an additive flame retardant with nylon 66 resin. However, for flame-retardant fibers, blended flame-retardant products are difficult to have better spinnability due to the high content of small-molecule flame retardants, and it is also difficult to obtain high fiber physical and mechanical properties, and flame retardants are used in spinning It is easy to precipitate during silk processing and product use, polluting the production environment, and the flame retardancy of the product will gradually decrease due to precipitation. [0003] It is an effective solution to obtain flame retardant nylon polymers by copolymerizing reactive flame retardants with nylon monomers. The flame ret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42
Inventor 杜选冯新星肖文华吴行姜立鹏
Owner LIAONING YINZHU CHEMTEX GROUP
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