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Preparation method for organic phosphorus copolymerized antiflaming polyamide material

A flame retardant and polyamide copolymerization technology, which is applied in the field of flame retardant materials, can solve the problems of large proportion of flame retardant, difficult viscosity of PA6, high cost of raw materials, etc., and achieve the effect of excellent flame retardant performance

Active Publication Date: 2014-12-24
JIANGSU RUIMEIFU IND
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Blending processing method, adding a large proportion of flame retardants, reduces the mechanical and electrical properties of polyamide itself; and cannot be used in the textile industry and film industry
[0005] At present, there are similar copolymerization processing methods, such as BASF, etc. (201180022888.3) introducing copolymerization flame retardant components with low polymerization efficiency, complicated process and high cost
[0006] The patent (201410056761.9) also discloses a scheme of flame retardant nylon. However, during the preparation of this scheme, all raw materials are added to the reactor at the same time for reaction, and a material with controllable viscosity cannot be obtained. The proportion of synergistic flame retardants, the cost of raw materials is high, and the viscosity of PA6 is difficult to control, and the proportion of flame retardant active ingredients is not high, making it difficult for the material to be used in the field of textiles and films

Method used

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  • Preparation method for organic phosphorus copolymerized antiflaming polyamide material
  • Preparation method for organic phosphorus copolymerized antiflaming polyamide material
  • Preparation method for organic phosphorus copolymerized antiflaming polyamide material

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preparation example Construction

[0047] A method for preparing an organophosphorus copolymerized flame-retardant polyamide material, specifically comprising the following steps:

[0048] (1) The flame retardant is reacted with the diamine monomer in advance to prepare a prepolymer.

[0049] Preferably, the flame retardant is or with is a derivative of the matrix;

[0050] where the R 1 and R 2 All are alkylene groups with 1-10 carbon atoms;

[0051] Or one of R1 and R2 is H; X 1 、X 2 H, or 1-4 halogens that can replace H on the benzene ring, such as Br, etc.

[0052] Preferably, the flame retardant and its derivatives are the following:

[0053] R1 is an alkylene group of 1-10 carbon atoms, R2 is H or an alkyl group of 1-10 carbon atoms;

[0054] R1 is an alkylene group of 1-10 carbon atoms, and R2 is an alkylene group of 1-10 carbon atoms;

[0055] R1 and R2 are each an alkylene group of 1-10 carbon atoms, and R3 is an alkyl group of 1-10 carbon atoms;

[0056] R1 and R3 are each an alkyle...

Embodiment 1

[0114] The flame retardant was reacted with hexamethylenediamine to obtain a mixture of No. 1 prepolymer and DDP hexamethylenediamine salt, and the molar ratio of flame retardant to hexamethylenediamine was 1:1.

[0115] Add caprolactam and a catalyst accounting for 1% of the weight of caprolactam into the reactor, vacuumize, fill with nitrogen, and maintain a positive pressure in the reactor; heat the reactor, control the temperature in the reactor to 240°C, and the pressure to 0.3MPa, then start stirring The device continued to stir for 8 hours; reduce the stirring speed, evacuate the reactor to a vacuum degree of -0.05MPa, and then fill it with nitrogen to normal pressure, and then add 1.5% prepolymer of caprolactam weight;

[0116] Vacuum again to -0.05MPa, keep the temperature in the reactor at 240°C, and carry out the copolymerization reaction for 15 minutes; finally fill in nitrogen, control the pressure in the reactor to 0.02MPa, discharge the material, cool, pelletize,...

Embodiment 2

[0119] The flame retardant is reacted with nonanediamine to obtain a mixture of No. 2 prepolymer and flame retardant nonanediamine salt, and the molar ratio of flame retardant to nonanediamine is 1:3.

[0120] Add caprolactam, undecanolactam, hexamethylenediamine with a mass ratio of 1:1:1 and a catalyst of 1% of the total weight of caprolactam, undecanolactam, and hexamethylenediamine into the reactor, vacuumize, fill with nitrogen, and keep The inside of the reactor is under positive pressure;

[0121] Heat the reaction kettle, control the temperature in the reaction kettle to 250°C and the pressure to 0.5MPa, start the stirring device and continue stirring for 7 hours; reduce the stirring speed, evacuate the reaction kettle to a vacuum degree of -0.04MPa and then fill it with nitrogen to normal pressure Add a prepolymer prepared by adding 2% flame retardant equivalent to the sum of the weight of lactam and diamine; evacuate again to a vacuum degree of -0.01MPa, keep the tem...

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Abstract

The invention relates to the field of antiflaming materials and particularly relates to a preparation method for an organic phosphorus copolymerized antiflaming polyamide material used for textile, engineering plastics and thin films. The preparation method of the organic phosphorus copolymerized antiflaming polyamide material specifically comprises the following steps: (1) enabling a fire retardant and a diamine monomer to react in advance to prepare a prepolymer; (2) adding a polymerized monomer, a catalyst and the prepolymer into a reaction kettle to prepare the organic phosphorus copolymerized antiflaming polyamide material. According to the organic phosphorus copolymerized antiflaming polyamide material provided by the invention, a small amount of the reaction fire retardant needs to be added, no synergic fire retardant is needed, the viscosity is controllable in the preparation process, the use property of the polymer finally obtained in the reaction is excellent, and the organic phosphorus copolymerized antiflaming polyamide material can be used in various fields of textile, engineering plastics, thin films and the like. Meanwhile, the use amount of raw materials is small, the process is simple, the cost is low, the actionability is high, and the flame retardant property of the prepared product is high.

Description

technical field [0001] The invention relates to the field of flame-retardant materials, in particular to a method for preparing an organophosphorus copolymerized flame-retardant polyamide material used in textiles, engineering plastics and films. Background technique [0002] Polyamide (such as PA6, PA66) has many excellent properties and is widely used in textiles, films, engineering plastics and other fields. However, polyamide itself is not flame retardant and can cause fires. Therefore, flame-retardant polyamides have always been a subject of research in the polyamide industry. [0003] At present, polyamide flame retardant is generally divided into two methods from the perspective of technology, one is to add flame retardants and related synergistic flame retardants after polyamide polymerization, and blend processing; the other is to add flame retardants and related synergistic flame retardants after polyamide polymerization; Introduce flame retardant components, cop...

Claims

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Application Information

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IPC IPC(8): C08G69/42
Inventor 杨纪财杨勇
Owner JIANGSU RUIMEIFU IND
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