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Permanent-flame-retardant nylon 6 material and preparation method therefor

A flame-retardant nylon, permanent technology, applied in the field of flame-retardant nylon synthesis, can solve the problems of small impact on performance, monotonous melting point, loss of fabric strength, etc., to achieve low flame retardant addition, high temperature performance, and mechanical properties small effect

Inactive Publication Date: 2015-12-16
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are three main methods for the flame retardant modification of polymer materials: first, the use of additive flame retardants. For nylon 6, flame retardants are mainly added to nylon 6 to achieve flame retardant modification. It is characterized by convenient use and wide application, but it has a great influence on the mechanical properties of materials
Second, use a reactive flame retardant, that is, the flame retardant participates in the reaction as a reactive monomer, and the flame retardant is combined with the main chain or side chain of nylon to make it have a flame retardant component. This method is less toxic , long-lasting flame retardant performance, and little impact on the performance of materials, but there are few types of reactive flame retardants, complex processing technology, and high cost. Currently, no additive flame retardants are commonly used
Third, flame retardant fabric finishing. Nylon 6 fabrics can obtain flame retardant effects by combining flame retardants with fabrics through flame retardant finishing, such as grafting, rolling baking, spray coating, etc. It is characterized by simple process, Easy to operate and flexible in processing, but may cause loss of fabric strength and affect its feel and washability
However, there are also shortcomings in the flame retardant modification of copolymerization. On the one hand, the introduction of flame retardants will inevitably affect the polymerization process of polymer materials, resulting in a decrease in molecular weight, which will inevitably affect its mechanical properties and affect its use effect; on the other hand , usually copolymerization flame retardant modification is to directly polymerize the flame retardant and nylon monomer to obtain a random copolymer of nylon and flame retardant. The flame retardant is randomly distributed in nylon. For random copolymers, with As the concentration of non-crystalline comonomer (flame retardant) increases, the melting point decreases monotonously. We are faced with the problem of not only needing a certain amount of flame retardant modification to obtain flame retardant nylon, but also maintaining the high temperature resistance of nylon. contradictory, which limits the use of nylon
In the modification of other polymers, there is no direct polycondensation, but the flame retardant is pretreated and crushed with the polymer material to block the polymer material during the blending process, and then the molecular weight is increased through solid-state polycondensation However, this method has disadvantages such as uneven distribution of flame retardants in polymer materials, low probability of flame retardants being bound to polymer main chains, and impact on the mechanical properties of materials.

Method used

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  • Permanent-flame-retardant nylon 6 material and preparation method therefor
  • Permanent-flame-retardant nylon 6 material and preparation method therefor
  • Permanent-flame-retardant nylon 6 material and preparation method therefor

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A preparation method of a permanent flame-retardant nylon 6 material, specifically comprising the following steps:

[0037] (1) Mix the flame retardant DDP, hexamethylenediamine and water, mix evenly at 50°C for 2 hours under the protection of nitrogen, then stir and react at 90°C for 2 hours, then raise the temperature to 150°C for further polymerization, and finally decompress and vacuumize, and react Finish generating flame retardant prepolymer, it is viscous liquid, number average molecular weight Mn is 1.8×10 3 , the molar ratio of flame retardant DDP, hexamethylenediamine and water is 1:1.1:2, and the two ends of the obtained flame retardant prepolymer are active end groups of a carboxyl group and an amine group respectively;

[0038] The structure of the flame retardant is:

[0039]

[0040] (2) 90.7 parts by mass of caprolactam, 4.0 parts by mass of water and 0.3 parts by mass of adipic acid are added to the reactor, and N 2 Exhaust the air in the kettle, s...

Embodiment 2

[0049] A preparation method of a permanent flame-retardant nylon 6 material, specifically comprising the following steps:

[0050] (1) Mix the flame retardant CEPPA, hexamethylenediamine and water, mix evenly at 80°C for 3 hours under the protection of nitrogen, then stir and react at 130°C for 3 hours, then raise the temperature to 180°C for further polymerization, and finally decompress and vacuumize, react Finish generating flame retardant prepolymer, it is semi-solid, number average molecular weight Mn is 2.5 * 10 3 , the molar ratio of flame retardant CEPPA, hexamethylenediamine and water is 1:1.2:2.5, and the two ends of the obtained flame retardant prepolymer are respectively a carboxyl group and an amine active end group;

[0051] The structure of the flame retardant is:

[0052]

[0053] (2) 84.0 parts by mass of caprolactam, 5 parts by mass of water and 1 part by mass of adipic acid are added to the reactor, and N 2 Exhaust the air in the kettle, stir at a speed...

Embodiment 3

[0062] A preparation method of a permanent flame-retardant nylon 6 material, specifically comprising the following steps:

[0063] (1) Mix the flame retardant BCPPO, hexamethylenediamine and water, mix evenly at 60°C for 2.5 hours under the protection of nitrogen, then stir and react at 95°C for 2 hours, then raise the temperature to 160°C for further polymerization, and finally vacuumize under reduced pressure, At the end of the reaction, a flame retardant prepolymer is generated, which is a viscous liquid with a number average molecular weight Mn of 2.8×10 3 , the molar ratio of flame retardant BCPPO, hexamethylenediamine and water is 1:1.2:2.1, and the two ends of the obtained flame retardant prepolymer are respectively a carboxyl group and an amine active end group;

[0064] The structure of the flame retardant is:

[0065]

[0066] (2) 92.9 parts by mass of caprolactam, 0.8 parts by mass of water and 0.8 parts by mass of adipic acid are added to the reactor, and N 2 ...

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Abstract

The invention relates to a permanent-flame-retardant nylon 6 material and a preparation method therefor and particularly relates to a preparation method for a block copolymerized flame-retardant nylon 6 material obtained through continuously and respectively carrying out two-step polymerization reaction on a phosphoric reactive flame retardant. The method is characterized by comprising the steps of firstly enabling the flame retardant to react with diamine or dibasic alcohol so as to obtain a flame retardant prepolymer, and then, enabling the flame retardant prepolymer to react and copolymerize with a prepolymer of nylon 6, thereby obtaining the permanent-flame-retardant nylon 6 material. The flame-retardant nylon 6 material prepared by the method has the characteristics of low flame retardant addition level and durable flame-retardant effect, the limiting oxygen index is over 30%, the vertical firing test reaches UL94V-0, and the mechanical properties are excellent; and the nylon 6 material can be subjected to injection molding directly or form films and can also become into fibers so as to further prepare flame-retardant fabrics.

Description

technical field [0001] The invention belongs to the technical field of flame retardant nylon synthesis, and relates to a permanent flame retardant nylon 6 material and a preparation method thereof, in particular to a prepolymerized material containing a flame retardant obtained by block copolymerization through continuous and separately carried out two-step polymerization reactions. A permanent flame-retardant nylon 6 material and a preparation method thereof. Background technique [0002] Nylon is one of the most important engineering plastics, and nylon 6 is the most widely used variety in nylon. Nylon 6 has excellent properties such as good wear resistance, deformation resistance, resilience and low temperature resistance, and can be made into fibers, films, engineering plastics, etc., but the limiting oxygen index of nylon 6 is 21-22%, and its flame retardancy is not good Ideal, severely limits the application of nylon 6. Therefore, it is of great significance to study...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42C09K21/14
Inventor 肖茹刘可李圆圆朱德振姜铭汉王华平
Owner DONGHUA UNIV
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