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Preparation method of unenhanced halogen-free flame retardant nylon 66

A technology of flame retardant nylon and flame retardant, applied in the field of preparation of non-reinforced halogen-free flame retardant nylon 66, which can solve the problems of high flame retardant grade, large addition amount, poor flame retardant effect, etc., and achieve excellent flame retardancy , high flame retardant effect

Active Publication Date: 2015-04-29
BEIJING CO FOUND HIGH TECH INCUBATOR
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Red phosphorus and melamine salts are the most widely used halogen-free flame retardant systems, but red phosphorus itself is colored and can only be used for black products, and generally only for nylon 6, with a narrow application range
In addition, there are melamine salts, mainly melamine uric acid salts and phosphates, but their flame retardant effect is not good, and the flame retardant effect formed is extremely unstable. Can only be used in occasions where flame retardancy requirements are not high

Method used

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

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preparation example Construction

[0017] The preparation method of non-enhanced halogen-free flame-retardant nylon 66 proposed by the present invention comprises the following steps:

[0018] (1) Synthetic halogen-free flame retardant:

[0019] Disperse acid chloride compounds and amines in toluene at a molar ratio of (1-3):1, stir at room temperature and heat to 90°C-110°C, reflux for 4-8 hours, and filter the reflux product Afterwards, dry in a stepwise heating manner, wash the product twice, filter, and dry the filtered product at 150°C for 3-5 hours to obtain a white halogen-free flame retardant, wherein the acyl chloride compound is benzoyl chloride, Any one of oxalyl chloride, acetyl chloride, terephthaloyl chloride, phthaloyl chloride, isophthaloyl chloride or trimesoyl chloride, and the amines mentioned are melamine, melamine cyanurate, melamine Any one of phosphate, melamine oxalate, melamine hydrochloride, aniline, p-phenylenediamine, ethylenediamine, hexamethylenediamine, 4,4'-diaminodiphenyl ether...

Embodiment 1

[0030] (1) Benzoyl chloride and melamine are dispersed in toluene at a molar ratio of 3:1, heated to 108°C after stirring at room temperature, and refluxed for 6 hours. Dry at 120°C for 1 hour, heat up to 150°C for 2 hours, heat up to 180°C for 2 hours, dry at 200°C for 2 hours, wash the product twice with water, filter and dry at 150°C for 5 hours to obtain white halogen-free Flame retardant 1, the yield is 90%.

[0031] (2) Set the temperature of the nylon slices at 105°C for constant temperature drying for 5 hours, and prepare the raw materials according to the following ratio:

[0032]

[0033] Add the above-mentioned raw materials to the high-speed mixer after weighing the above-mentioned parts by weight and mix evenly;

[0034] (3) Preheat the twin-screw extruder, and set the temperatures of the conveying section, melting section, extrusion section, exhaust section and shear section to 260°C, 275°C, 275°C, 270°C and 265°C respectively , keep warm for 30 minutes afte...

Embodiment 2

[0036] (1) Oxalyl chloride and melamine oxalate were dispersed in toluene at a molar ratio of 1.5:1, heated to 98°C after stirring at room temperature, and refluxed for 5 hours. After filtering the refluxed reaction product, it was dried in a stepwise heating manner. That is, the temperature was raised to 120°C for 1 hour, the temperature was raised to 150°C for 2 hours, the temperature was raised to 180°C for 2 hours, and the temperature was raised to 200°C for 2 hours. Halogen-free flame retardant 2, the yield is 92%.

[0037] (2) Set the temperature of the nylon slices at 105°C for constant temperature drying for 5 hours, and prepare the raw materials according to the following ratio:

[0038]

[0039] Add the above-mentioned raw materials to the high-speed mixer after weighing the above-mentioned parts by weight and mix evenly;

[0040](3) Preheat the twin-screw extruder, and set the temperatures of the conveying section, melting section, extrusion section, exhaust sec...

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Abstract

The invention relates to a preparation method of an unenhanced halogen-free flame retardant nylon 66, and belongs to the technical field of flame retardant engineering plastics. The method comprises the following steps: synthesizing a halogen-free flame retardant; preparing raw materials according to the following proportions: 65-85 parts by weight of nylon 66 sliced sections, 8-20 parts of self-synthesized halogen-free flame retardant, 1-5 parts of auxiliary flame retardant, 0-2.5 parts of compatilizer, 0.5-2 parts of flexibilizer, 0.5-1.5 parts of silane coupling agent, 1-4 parts of antioxygen; adding the materials into a high-speed mixing machine to uniformly mix; melting and extruding; feeding a mixture into a double-screw extruder for melting, blending and extruding; bracing; water-cooling; and chopping and drying to obtain the flame retardant nylon 66. The prepared flame retardant nylon is high in flame retardance, high in toughness, high in abrasion resistance, high in electric performance, high in heat resistant performance and the like; based on a complex synergistic effect of the self-synthesizing flame retardant and the auxiliary flame retardant, a good and stable effect can be realized, and the preparation method can be widely suitable for the fields of automobiles, mechanical industries, electronic appliances, precise instruments and the like.

Description

technical field [0001] The invention relates to a preparation method of non-reinforced halogen-free flame-retardant nylon 66, which belongs to the technical field of flame-retardant engineering plastics. Background technique [0002] With the rapid development of the electrical and electronic industry and other special industries, the flame retardancy of unmodified nylon is poor, and its vertical combustion can only reach UL94V-2 level, the oxygen index is about 24, and it produces droplets during the combustion process. Falling is a flammable material. It is very easy to cause fires during use, especially in the field of electronic products. There are countless fires caused by nylon, causing great losses. [0003] At present, there are many kinds of flame retardants used in nylon 66, including: brominated flame retardants such as decabromodiphenyl ether, decabromodiphenylethane, etc.; phosphorus-based flame retardants such as red phosphorus; nitrogen-based flame retardants...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L77/06C08K13/02C08K5/3492C08K5/20C08K5/17C08K3/22C08K3/36C08K3/38B29C47/92B29C48/92
CPCB29C48/92C08K3/2279C08K5/09C08K5/1345C08K5/3492C08K13/02C08L77/06C08L2201/02C08L2201/22C08L2205/02C08L2205/03C08L47/00C08L63/00C08K5/12C08L67/02C08K3/38C08L77/00C08L77/02
Inventor 尹继磊钱志国毕立高纬婧孙洁郭雪山钱毅李正梅边策杨慧竺朝山孙玉增成文刚王立新朱朗晖
Owner BEIJING CO FOUND HIGH TECH INCUBATOR
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