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Phosphorus nitrogen intumescent flame retardant and its preparation method and use

An intumescent flame retardant, phosphorus-nitrogen technology, applied in the field of flame-retardant materials, can solve the problems of poor thermal stability, poor polymer compatibility, low molecular weight of phosphorus-nitrogen flame retardants, etc., to improve flame retardant performance , large molecular weight, good thermal stability

Active Publication Date: 2019-06-07
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Nowadays, the synthesis of phosphorus-nitrogen flame retardants has become an important research topic, but most of the phosphorus-nitrogen flame retardants have low molecular weight, poor thermal stability and poor compatibility with polymers, and are easy to process during processing. Precipitation and decomposition, so in order to obtain polycaprolactam materials with better performance, synthesizing macromolecular flame retardants is also a good solution

Method used

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  • Phosphorus nitrogen intumescent flame retardant and its preparation method and use
  • Phosphorus nitrogen intumescent flame retardant and its preparation method and use
  • Phosphorus nitrogen intumescent flame retardant and its preparation method and use

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Embodiment 1

[0030] This embodiment relates to a preparation method of a phosphorus-nitrogen intumescent flame retardant, which comprises the following steps:

[0031] Dissolve 0.03mol of terephthalaldehyde in 80mL of absolute ethanol to obtain a reaction solution, add it to a 500mL three-neck flask, then blow in nitrogen and raise the temperature to 60°C, dissolve 0.03mol of DDM in 80mL of absolute ethanol, and turn on the magnetic stirring The device was stirred at a speed of 300rpm, and then added dropwise to the above reaction solution, heated to reflux temperature and continued to react for 4 hours, then cooled to room temperature, and then 0.06mol DOPO dissolved in 100mL of absolute ethanol was slowly added dropwise to the above After reacting in the solution for one hour, raise the temperature to reflux temperature and continue to react for 8 hours, take it out, wash, dry and grind to obtain yellow powder of high-efficiency phosphorus-nitrogen expansion flame retardant.

[0032] The...

Embodiment 2

[0034] This embodiment relates to a preparation method of the phosphorus-nitrogen intumescent flame retardant flame-retardant polycaprolactam obtained in Example 1, which comprises the following steps:

[0035] The flame retardant accounting for 10% of the total mass percentage of flame-retardant polycaprolactam and the polycaprolactam accounting for 90% are put into a mixer and mixed uniformly, and then the flame retardant and polycaprolactam resin are melt-blended, injected, cooled, and cut. After pelleting, flame-retardant polycaprolactam pellets with a flame-retardant grade of UL94V-1 (3.2mm) can be obtained.

Embodiment 3

[0037] This embodiment relates to a preparation method of the phosphorus-nitrogen intumescent flame retardant flame-retardant polycaprolactam obtained in Example 1, which comprises the following steps:

[0038] The flame retardant accounting for 15% of the total mass percentage of flame-retardant polycaprolactam and the polycaprolactam accounting for 85% are put into a mixer and mixed uniformly, and then the flame retardant and polycaprolactam resin are melt-blended, injected, cooled, and cut. After granulation, the flame-retardant polycaprolactam pellets with a flame-retardant grade of UL94V-0 (3.2mm) can be obtained.

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Abstract

The invention discloses a preparation method of an efficient phosphorus and nitrogen intumescent flame retardant and an application of the phosphorus and nitrogen intumescent flame retardant to polycaprocactam. The preparation method comprises the steps: carrying out condensation reaction on p-phthalaldehyde and 4,4'-methylenedianiline (DDM), and then, carrying out addition reaction on the product and DOPO to obtain solid nitrogen and phosphorus containing flame retardant molecules; and then, uniformly mixing the obtained flame retardant with polycaprolactam resin, and carrying out melt blending at 220-260 DEG C to obtain a halogen-free flame retardant polycaprolactam material. The method is capable of realizing synthesis at one step without separating intermediate products, simple in synthesis process, simple and convenient in aftertreatment, high in efficiency, safe, environment-friendly and convenient to realize industrial mass production; and the flame retardant belongs to a polymer-type flame retardant, contains a carbon source, an acid source and a nitrogen source, does not contain halogens and is nontoxic, pollution-free, green and environment-friendly, polycaprolactam reaches the UL94V-0 level when the addition amount of the flame retardant is 15%, and the mass percentage of residues is 37.8% at 700 DEG C.

Description

technical field [0001] The invention relates to a phosphorus-nitrogen intumescent flame retardant, a preparation method and application thereof, and belongs to the technical field of flame-retardant materials. Background technique [0002] At present, with the advancement of science and technology and the widespread use of polymer materials, people's requirements for flame retardant materials are gradually increasing, especially since July 1, 2006, the EU ROHS has banned the use of Due to the sales of electronic and electrical products of polybrominated diphenyl ethers and polybrominated biphenyls that produce dioxins, the application of such halogen-containing flame-retardant materials has been greatly restricted, and their products are gradually losing their market competitiveness. [0003] Nylon is one of the earliest and most widely used engineering plastics, and polycaprolactam is the most widely used material in nylon materials. Therefore, it is particularly important ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G12/40C08G12/06C08L77/02C08L61/32
CPCC08G12/06C08G12/40C08L77/02C08L2201/02C08L2201/08C08L2201/22C08L61/32
Inventor 任亮李中诚张明耀韩业邵珠宝
Owner CHANGCHUN UNIV OF TECH
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