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Halogen-free copolymer-type flame-retarding polyamide 66 and preparation method thereof

A flame-retardant polyamide, copolymerization technology, applied in the field of halogen-free copolymerization flame-retardant polyamide 66 and its preparation, can solve the problem of loss of material application performance, branching, reticulation, inability to form long-chain polymers, etc. question

Active Publication Date: 2016-05-18
LIAONING YINZHU CHEMTEX GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the actual control process of the above reaction, since the molecular structure of the phosphorus-containing flame retardant itself contains one or more benzene ring structures, it is easy to cause polyamide 66 reaction during the reaction process of polyamide 66, especially in the initial stage of the reaction. The branching and reticulation of polyamide 66 can not form long-chain polymers in the subsequent post-polymerization process or in the remelting process of fiber formation and casting.
Such a flame-retardant polyamide 66 material loses the application performance of the material itself during the application process

Method used

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  • Halogen-free copolymer-type flame-retarding polyamide 66 and preparation method thereof
  • Halogen-free copolymer-type flame-retarding polyamide 66 and preparation method thereof
  • Halogen-free copolymer-type flame-retarding polyamide 66 and preparation method thereof

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preparation example Construction

[0021] The preparation of the halogen-free copolymerized flame-retardant polyamide 66 of the present invention is carried out according to the following steps:

[0022] (1) Preparation of the flame retardant organic salt solution: the organophosphorus flame retardant and the hexamethylenediamine solution with a concentration of 25 to 35wt.% are mixed to react to generate the flame retardant organic salt solution; The molar ratio of amines is 1:1.

[0023] (2) Pre-amidation reaction of hexamethylenediamine and adipic acid: mix hexamethylenediamine and adipic acid in the polymerization tank at a molar ratio of 1:1, control the pressure in the polymerization tank to 1.75-2.0MPa, and the temperature to 210- At 250°C, under this condition, hexamethylenediamine and adipic acid undergo a pre-amidation reaction, and the reaction time is 2-3 hours to obtain polyamide 66.

[0024] (3) After the step (2) pre-amidation reaction, the pressure in the polymerization tank is reduced to norma...

Embodiment 1

[0026] 1, get CEPPA3kg, hexamethylenediamine 0.81kg, be mixed with the flame retardant organic salt solution of concentration 60wt% (according to the amount calculation of corresponding CEPPA), pH value 7.5, reaction formula is as follows formula (1):

[0027]

[0028] 2. Add 200kg of nylon 66 (1:1 molar ratio of hexamethylenediamine to adipic acid) salt solution in a 300L polymerization kettle, the concentration is 50wt.%, the pressure is 1.75MPa, the temperature is 250°C, and the pre-amidation reaction is completed after 150min , to obtain polyamide 66.

[0029] 3. After the pressure of the polymerization tank where the reaction in step 2 is completed is reduced to -0.05MPa, inject the flame retardant organic salt solution prepared in step 1 into it. At a temperature of 284°C, the polymerization reaction is completed after 30 minutes to obtain halogen-free copolymerization Type flame-retardant polyamide 66 polymer material (slice), the reaction formula is as follows (2): ...

Embodiment 2

[0036] 1, get DDP4.5kg, hexamethylenediamine 1.5kg, be mixed with concentration 60wt% (according to the amount calculation of corresponding DDP), the flame retardant organic salt solution that pH value is 7.1, reaction formula is as follows formula (3):

[0037]

[0038]2. Add 200kg of nylon 66 salt solution to the 300L polymerization kettle, nylon 66 (1:1 molar ratio of hexamethylenediamine adipic acid) salt solution, the concentration is 50wt.%. Amidation reaction to obtain polyamide 66.

[0039] 3. After the pressure of the polymerization tank that completed the reaction in step 2 was reduced to -0.05MPa, inject the flame retardant organic salt solution prepared in step 1 into it. At a temperature of 284°C, the polymerization reaction was completed after 30 minutes to obtain halogen-free copolymerization Type flame-retardant polyamide 66 polymer material (slice), the reaction formula is as follows (4):

[0040]

[0041] The flame retardant polyamide 66 infrared absor...

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Abstract

The invention discloses halogen-free copolymer-type flame-retarding polyamide 66 and a preparation method thereof and belongs to the technical field of flame-retarding polyamide 66 high-molecular materials. The method includes the steps of 1) preparing a flame retardant organic salt solution; 2) mixing hexanediamine and adipic acid in a polymerization kettle, and carrying out a pre-amidation reaction to prepare polyamide 66; 3) when the pre-amidation reaction is finished, reducing the pressure in the polymerization kettle to normal or negative pressure through flash pressure reduction, and adding the flame retardant organic salt solution to the polyamide 66 in the polymerization kettle, and performing after-polymerization reaction under a normal or negative pressure to prepare the halogen-free copolymer-type flame-retarding polyamide 66. The halogen-free copolymer-type flame-retarding polyamide 66 is not subjected to a thermal pyrolysis reaction in a remelting process during fiber forming and casting processes. The active component in the halogen-free copolymer-type flame-retarding polyamide 66 is phosphorus in a low content so that the flame-retarding efficiency is high.

Description

technical field [0001] The invention relates to the technical field of flame-retardant polyamide 66 polymer materials, in particular to a halogen-free copolymerization type flame-retardant polyamide 66 and a preparation method thereof. Background technique [0002] Polyamide 66 is relatively flammable, and its limiting oxygen index (LOI), an important indicator of flame retardancy, is 24. The traditional flame retardant polyamide 66 is added to the polyamide 66 matrix by means of physical blending and other methods. There is no chemical reaction between the flame retardant and polyamide 66, and there is no chemical bond combination. It is just a mixed Dispersal process. The disadvantage of this kind of flame-retardant polyamide 66 is that the blend system is prone to microscopic phase separation, which destroys the mechanical properties of the material and limits its application. This blended flame-retardant polyamide 66 cannot be applied to the main application field of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42C08G69/26
Inventor 杜选吴行邹琳姜立鹏杨贺于波徐洁薛小翠李天昌
Owner LIAONING YINZHU CHEMTEX GROUP
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