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A kind of high-viscosity flame-retardant polyamide 6 and preparation method thereof

A flame retardant polyamide and high viscosity technology, applied in the field of flame retardant preparation, can solve the problem of low viscosity of copolymerized flame retardant polyamide, and achieve the effect of overcoming low temperature resistance

Active Publication Date: 2020-02-14
THE QUARTERMASTER EQUIP INST OF THE LOGISTICAL SUPPORT DEPT CMC
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a high-viscosity flame-retardant polyamide 6 and its preparation method to solve the problem of low viscosity of copolymerized flame-retardant polyamide

Method used

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  • A kind of high-viscosity flame-retardant polyamide 6 and preparation method thereof
  • A kind of high-viscosity flame-retardant polyamide 6 and preparation method thereof
  • A kind of high-viscosity flame-retardant polyamide 6 and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, high-viscosity flame-retardant polyamide 6

[0045] 1. Preparation of flame retardant prepolymer:

[0046] 1.1) Mix the flame retardant CEPPA, ethylenediamine, ethylene glycol and water in a ratio of 1:1.1:1:100 (mol), and the mixing time is 0.5h;

[0047] 1.2) After mixing evenly, stir and react for 1 hour under nitrogen protection at a temperature of 50°C;

[0048] 1.3) After the stirring reaction, pressurize to 0.2MPa, and further raise the temperature to 180°C under the protection of nitrogen to carry out the polymerization reaction, and prepare the flame retardant prepolymer after reacting for 1 hour;

[0049] 1.4) The weight average molecular weight of the prepared flame retardant prepolymer is 2000.

[0050] 2. Preparation of high viscosity flame retardant polyamide 6

[0051] 2.1) Melting and mixing caprolactam and deionized water, the amount of water accounts for 4% of the whole weight;

[0052] 2.2) Raise the temperature of the molten reactan...

Embodiment 2

[0057] Embodiment 2, high-viscosity flame-retardant polyamide 6

[0058] 1. Preparation of flame retardant prepolymer:

[0059] 1.1) Mix the flame retardant DDP, ethylenediamine, ethylene glycol and water at a ratio of 1:1.2:1:50 (mol), and the mixing time is 1h;

[0060] 1.2) After mixing evenly, stir and react under nitrogen protection at 90°C for 1 hour;

[0061] 1.3) After stirring and reacting, pressurize to 0.2MPa, and further raise the temperature to 190°C under the protection of nitrogen to carry out polymerization reaction, and prepare the flame retardant prepolymer after reacting for 2 hours;

[0062] 1.4) The weight average molecular weight of the prepared flame retardant prepolymer is 3000.

[0063] 2. Preparation of high viscosity flame retardant polyamide 6

[0064] 2.1) Melting and mixing caprolactam and deionized water, the amount of water accounts for 5% of the whole weight;

[0065] 2.2) Raise the temperature of the molten reactant to 230°C for reaction, th...

Embodiment 3

[0070] Embodiment 3, high-viscosity flame-retardant polyamide 6

[0071] 1. Preparation of flame retardant prepolymer:

[0072] 1.1) Mix the flame retardant DDP sodium salt, propylenediamine, propylene glycol and water at a ratio of 1:1.15:1:70 (mol), and the mixing time is 0.5h;

[0073] 1.2) After mixing evenly, stir and react under nitrogen protection at 55°C for 1 hour;

[0074] 1.3) After stirring and reacting, pressurize to 0.2MPa, and further raise the temperature to 182°C under the protection of nitrogen to carry out polymerization reaction, and prepare the flame retardant prepolymer after reacting for 1.5h;

[0075] 1.4) The weight average molecular weight of the prepared flame retardant prepolymer is 2500.

[0076] 2. Preparation of high viscosity flame retardant polyamide 6

[0077] 2.1) Melting and mixing caprolactam and deionized water, the amount of water accounts for 4% of the whole weight;

[0078] 2.2) Raise the temperature of the molten reactant to 210°C ...

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Abstract

The invention discloses a high-viscosity flame retardant polyamide 6 and a preparation method thereof. The preparation method of the high-viscosity flame retardant polyamide 6 comprises the following steps: in water, a flame retardant containing phosphorus, a diamine and a dihydric alcohol are subjected to a pre-polymerization reaction, a polymerization reaction is performed, and therefore a flame retardant prepolymer is obtained; and the flame retardant prepolymer is added in a polyamide 6 polymerization process, and therefore the high-viscosity flame retardant polyamide 6 is obtained. In the prior art, a flame retardant is added, problems that temperature resistance is low, steric hindrance is large, effects are large and the like exist in a in-situ polymerization flame retardant polyamide 6, so that the current flame retardant polyamide 6 is low in viscosity, difficult in polymerization and even pelletizing cannot be performed, and the current flame retardant polyamide 6 is not suitable for spinning or phenomena such as a large number of floating silk and the like exist in the spinning. According to the invention, through the method of preparing the flame retardant prepolymer firstly through a pre-polymerization reaction, a problem that the flame retardant has the low temperature resistance is overcome, in middle and later periods of a polymerization process, the flame retardant prepolymer is added, thus a problem that polymer viscosity is low because the flame retardant is added in an early period, the viscosity is up to 2.8-3.2 Pa.s, and the high-viscosity flame retardant polyamide 6 is successfully prepared.

Description

technical field [0001] The invention relates to a high-viscosity flame-retardant polyamide 6 and a preparation method thereof, belonging to the field of flame retardant preparation. Background technique [0002] As one of the most important engineering plastics and textile fiber materials, polyamide has many excellent properties such as high strength and wear resistance, and is widely used in construction, textile, military and other fields. However, the flammability of polyamide affects its wider application. At present, most of the development of flame retardant polyamide still stays in the blending and granulation of polyamide matrix and blended flame retardants and related synergistic flame retardants. This method has many disadvantages such as adding a large amount of flame retardants, The poor dispersion in the polyamide matrix and the limitation of many properties of the polyamide itself have narrowed the application range of the blended flame retardant polyamide. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/42C08G69/36
CPCC08G69/36C08G69/42
Inventor 冯新星张华王修行来侃张长琦潘凯
Owner THE QUARTERMASTER EQUIP INST OF THE LOGISTICAL SUPPORT DEPT CMC
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