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Method for preparing halogen free flame-retarded nylon 6

A technology of flame-retardant nylon and mass parts, which is applied in the field of preparation of halogen-free flame-retardant nylon 6, which can solve the problems of increasing the cost of raw materials for users, only being used in the plastics industry, and increasing the manufacturing cost of flame-retardant nylon 6.

Active Publication Date: 2010-09-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] When preparing flame-retardant nylon 6 in the prior art, due to the large amount of flame retardant added, the fine flame retardant is easy to agglomerate to form a stress concentration point during the processing, and the nylon 6 body resin is heated through the secondary processing of the screw. Therefore, The mechanical properties of the material are much lower than that of pure nylon 6, so it can only be used in the plastic industry; at the same time, due to the increase of the follow-up screw process, the manufacturing cost of flame-retardant nylon 6 has also increased to a certain extent, thus directly increasing the cost of raw materials for users

Method used

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  • Method for preparing halogen free flame-retarded nylon 6

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: In a 10-liter polymerization kettle, 2.9 parts of adipic acid and 2.47 parts of melamine were added and stirred for 3 hours at 50° C., then centrifugally filtered, and the prepared adipate melamine salt and 2.3 parts of hexamethylenediamine were dried. Stir and react with 2.53 parts of cyanuric acid at 80°C for 0.5 hours, then centrifuge and filter, dry the prepared two flame-retardant monomers of hexamethylenediamine cyanurate, 1 part of pentaerythritol, and 0.01 part of tungstic acid. The substance is pre-dispersed and mixed with a high-shear emulsifier, 88.79 parts of molten caprolactam, and 0.3 part of water, and then heated to 230-265°C and stirred for 5 hours under a pressure of 0.2-0.8 MPa. Vacuum removal of low-molecular weight, discharge casting tape pelletization, and obtain halogen-free flame-retardant nylon 6 particles. After extraction and drying, samples are obtained for flame-retardant and mechanical performance testing. The results are shown i...

Embodiment 2

[0035] Example 2: In a 10-liter polymerization kettle, put 2.47 parts of melamine, 2.53 parts of cyanuric acid, 5.2 parts of nylon 66 salt, 1 part of pentaerythritol, and 0.01 part of tungstic acid. Pre-disperse and mix molten caprolactam and 0.3 parts of water, then raise the temperature to 230-265°C, and stir the polymerization reaction for 8 hours at a pressure of 0.2-0.8 MPa, then release the pressure, decompress and vacuumize to remove low molecules, and discharge the material to cast and cut into pellets , the obtained halogen-free flame-retardant nylon 6 particles were extracted and dried, and the samples were obtained for flame-retardant and mechanical performance testing. The results are shown in Table 1.

Embodiment 3

[0036] Embodiment 3: first in the colloid mill, drop into by 2.9 parts of adipic acid and 2.47 parts of melamine at 95 DEG C and stir and react for 1.5 hours, then centrifuge and filter, dry the prepared melamine adipate, 2.3 parts of hexamethylenediamine and 2.53 parts of cyanuric acid were stirred and reacted at 50°C for 2 hours, then centrifugally filtered, and dried to obtain two flame-retardant monomers composed of hexamethylenediamine cyanurate, 1 part of pentaerythritol, 0.01 part of tungstic acid and 88.79 parts The molten caprolactam and 0.3 parts of water are pre-dispersed and mixed; then the pre-dispersed mixed solution is pumped into the polymerization tank, the temperature is raised to 230-265 ° C, and the pressure is 0.2-0.8 MPa to stir the polymerization reaction for 5-8 hours, and then unload Pressure, decompression and vacuum pumping to remove low molecular weight, discharge material, cast belt and cut pellets to obtain halogen-free flame-retardant nylon 6 part...

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Abstract

The invention provides a method for preparing halogen-free flame retardant nylon 6. Dicarboxylic aid melamine salt, organic diamine cyanuric acid salt or melamine, cyanuric acid, acylamide salt, carbon forming agent, carbonization accelerant, caprolactam and water are added into a reactor, are dispersed and are mixed; the mixture is heated to a temperature of between 230 and 265 DEG C, is stirred, is subjected to polymerization reaction for 5 to 8 hours at a pressure of between 0.2 MPa and 0.8 MPa, and is subjected to pressure relief, decompression, vacuumization and low molecule removal to obtain the halogen-free flame retardant nylon 6. The material prepared by the method has good stability and little toxicity, substantially improves mechanical performance, has lasting flame retardance and can be directly used for flame-retardant yarn or engineering plastic.

Description

technical field [0001] The invention relates to a preparation method of halogen-free flame-retardant nylon 6 Background technique [0002] The flame retardant modification of nylon 6 is not only the focus of engineering plastics research, but also has always been a frontier subject in the field of textile research. In many studies, although PA6 fiber can achieve flame retardancy, most of them use halogen-containing or phosphorus-containing flame retardants to blend with PA6 matrix resin or to achieve flame retardancy through surface treatment in the fabric finishing process; halogen-free The research and production of flame-retardant PA6 plastics are also limited to screw blending. [0003] The method used in the preparation of the above-mentioned flame-retardant nylon 6 engineering plastics is screw blending; due to the large amount of flame retardant added, the fine flame retardants are easy to agglomerate during processing to form stress concentration points, and at the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/14C08G69/16C08K5/3492
Inventor 夏金魁熊远凡伍仟新姚亮红黄桂梅董维权丁小媛
Owner CHINA PETROLEUM & CHEM CORP
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