Reaction type nylon flame retardant and preparation method

A flame retardant and reactive technology, applied in the field of flame retardants, can solve the problems of a large amount of harmful smoke and corrosive gas, other performance degradation of composite materials, and color deterioration of composite materials, and achieve high practical value and high phosphorus content , the effect of stable quality

Active Publication Date: 2015-01-28
CHENGDU TALY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High energy consumption and serious environmental pollution. When halogenated flame retardants are burned, a large amount of harmful smoke and corrosive gases are produced, causing serious pollution to the environment.
The cost of flame retardant is high, the process control is complicated, and it is difficult to industrialize production
The addition of flame retardants leads to the decline of other properties of the composite material, and also makes the color of the composite material worse, affecting its application

Method used

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  • Reaction type nylon flame retardant and preparation method
  • Reaction type nylon flame retardant and preparation method
  • Reaction type nylon flame retardant and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Take 1.8Kg of ethylene glycol and 2.5Kg of hydroxymethylphenyl hypophosphorous acid into the reaction kettle, raise the temperature to 80°C, blow in nitrogen, esterify at 150°C for 3~5h, then at 170°C, -0.02~-0.096MPa Reaction under reduced pressure for 3~6 hours, the esterification rate is above 99%, and when no distillate is produced, stop the reaction, lower the temperature to 120°C, and discharge the material to obtain a flame-retardant esterification liquid, which is cooled for later use.

[0055] Take 2.2Kg of flame-retardant esterification liquid and 0.6Kg of malonic acid into the reaction kettle, raise the temperature to 80°C, blow in nitrogen, stir well, and esterify at 150°C for 3h~5h, then at 170°C, -0.02~ Reaction under reduced pressure at -0.096MPa for 3~6h. When no distillate is produced, stop the reaction, lower the temperature to 120°C, and discharge the material to obtain a reactive nylon flame retardant.

Embodiment 2

[0057] Take 3.1Kg of ethylene glycol and 4.8Kg of hydroxyethylphenyl hypophosphorous acid into the reaction kettle, raise the temperature to 80°C, blow in nitrogen, esterify at 80°C for 3~5h, then at 150°C, -0.02~-0.096MPa Reaction under reduced pressure for 3~6 hours, the esterification rate is above 99%, and when no fraction is produced, stop the reaction, lower the temperature to 100°C, and discharge the material to obtain a flame-retardant esterification liquid, which is cooled for later use.

[0058] Take 6.2Kg of flame retardant esterification liquid and 1.6Kg of malonic acid into the reaction kettle, raise the temperature to 80°C, blow in nitrogen, stir well, esterify at 80~150°C for 3~5h, then at 150°C, - Reaction under reduced pressure at 0.02~-0.096MPa for 3~6h, when no distillate is produced, stop the reaction, lower the temperature to 100°C, and discharge the material to obtain a reactive nylon flame retardant.

Embodiment 3

[0060] Take 1.8Kg of ethylene glycol and 3.1Kg of 2-carboxyethylphenyl hypophosphorous acid and add them into the reaction kettle, raise the temperature to 80°C, feed in nitrogen, stir well, and gradually heat up after the 2-carboxyethylphenylphosphorous acid is completely dissolved. Esterify at 140°C for 3~5h, then react under reduced pressure at 160°C and -0.02~-0.096MPa for 3~6h, the esterification rate is above 99%, stop the reaction when no fraction is produced, and lower the temperature to 110°C , discharging, to obtain a flame retardant esterified liquid, cooled for subsequent use.

[0061] Take 3.8Kg of flame retardant esterification solution and 1.5Kg of adipic acid into the reaction kettle, raise the temperature to 80°C, blow in nitrogen, stir well, and esterify at 140°C for 3~5h, then at 160°C, -0.02~ Reaction under reduced pressure at -0.096MPa for 3-6h. When no distillate is produced, stop the reaction, lower the temperature to 110°C, and discharge the material to...

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Abstract

The invention belongs to the field of flame retardants, and especially relates to a reaction type nylon flame retardant and a preparation method. The technical scheme is characterized in that the halonge-free phosphorus-containing nylon flame retardant is synthesized by a two-step process, a first step is preparation of a flame-retardation esterification liquid, the formula comprises 5-52 parts by mass of a halogen-free phosphorus-containing copolymerization type flame retardant and 20-65 parts of a dihydric alcohol, and the flame-retardation esterification liquid is obtained by reacting the above two compositions under a certain condition; and a second step is preparation of the halogen-free phosphorus-containing nylon flame retardant, based on the mass quantity of the flame-retardation esterification liquid, the formula comprises 18-60 parts of the flame-retardation esterification liquid and 5-48 parts of a dibasic acid, and the halogen-free phosphorus-containing nylon flame retardant is obtained by reacting the above two compositions under a certain condition. The obtained flame retardant is resistant to a high temperature of 250 DEG C, satisfies the polymerization temperature of nylon, is polymerized onto a nylon molecular chain in a monomer form in a nylon polymerization process, and has persistent flame retardation effect. The prepared nylon flame retardant has the limit oxygen index of 30% or more, has excellent flame retardation performance, is applicable to produce flame-retardant nylon with the flame retardation performance of UL94V-0 grade or more, and is an efficient environment-friendly nylon flame retardant.

Description

technical field [0001] The invention belongs to the field of flame retardants, in particular to a reactive nylon flame retardant and a preparation method thereof, which can be used as a reactive flame retardant or as an additive flame retardant, and can be used to produce flame retardants up to UL94 V- Grade 0 flame retardant nylon. [0002] Background technique [0003] Nylon (PA) is a general term for thermoplastic resins containing repeating amide groups on the molecular backbone. In 1930, the DuPont Company of the United States first launched PA. So far, PA has developed into a class of engineering plastics with the most varieties, the largest output, and the most widely used in the world. While PA brings comfort and convenience to people, its flammability also brings potential fire hazards. Therefore, under the premise of maintaining the mechanical properties of PA, it is necessary to further improve its flame retardancy, electrical properties, processing properties,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C08L77/00C07F9/32
Inventor 张先银汪丹吴行陈群跃黄旭陶云峰方辉
Owner CHENGDU TALY TECH CO LTD
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