A kind of halogen-free anti-droplet flame-retardant nylon 6 resin and preparation method thereof

A flame-retardant nylon and anti-droplet technology, which is applied in the field of flame-retardant resin and its preparation, can solve the problems of the decline in mechanical properties of nylon 6 materials and the large amount of flame retardant added, and achieve good and longer-lasting flame-retardant effects, flame-retardant high efficiency effect

Active Publication Date: 2019-07-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] It can be seen that currently in the field of flame retardant nylon 6, flame retardants are added to nylon 6 flame retardant products in the form of copolymerization, usually with phosphate as the main body of flame retardants, nitrogen-based, silicon-based, metal and other flame retardants As an auxiliary flame retardant material, however, phosphorus-based flame retardants will produce toxic intermediate products such as phosphoric acid and metaphosphoric acid during combustion, which will inevitably have a negative impact during use.
For flame retardant materials prepared by blending, in order to achieve a better flame retardant effect, the addition of flame retardants is relatively large, which will inevitably cause a significant decline in the mechanical properties of nylon 6 materials.

Method used

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  • A kind of halogen-free anti-droplet flame-retardant nylon 6 resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (a) Preparation of green and environmentally friendly silicon-based flame-retardant oligomers

[0041] Weigh 10 g of diphenylsilanediol (DPSD), 0.135 g of HCl and 50 ml of tetrahydrofuran (THF) and fully dissolve them in a three-necked flask. Stir under the conditions of 25° C. and 800 Pa, and react for 60 hours. After the reaction is complete, the product polyphenylsiloxane (PDPS, m≈4) is obtained.

[0042] (b) Preparation of Nylon 6 Ester

[0043] Step 1: Add 100g of caprolactam, 5g of water, 1g of aminocaproic acid and 16.75g of adipic acid into the reaction kettle, pass nitrogen gas 3 times until the air in the kettle is replaced, and maintain a pressure of 0.025MPa, then raise the temperature to 260 ℃, stirred and reacted for 2 hours; the pressure in the kettle was adjusted to 400Pa, and the reaction was continued at 220℃ for 2 hours to obtain a carboxylated PA6 prepolymer with a molecular weight of 1000.

[0044] Step 2: After the reaction in the first step is c...

Embodiment 2

[0048] (a) Preparation of green and environmentally friendly silicon-based flame-retardant oligomers

[0049] Weigh 10g diphenylsilanediol (DPSD), 0.18g H 2 SO 4and 50ml of N,N dimethylpyrrolidone (NMP) were fully dissolved in a three-neck flask. Stir under the conditions of 80° C. and 200 Pa, and react for 8 hours. After the reaction is complete, the product polyphenylsiloxane (PDPS, m≈4)) is obtained.

[0050] (b) Preparation of Nylon 6 Ester

[0051] Step 1: Add 100g of caprolactam, 2g of water, 4g of aminocaproic acid and 7.8g of adipic acid into the reaction kettle, pass nitrogen gas 3 times until the air in the kettle is replaced, and maintain a pressure of 0.2MPa, then raise the temperature to 260 ℃, stirred and reacted for 2 hours; the pressure in the kettle was adjusted to 200Pa, and the reaction was continued at 240℃ for 2 hours to obtain a carboxylated PA6 prepolymer with a molecular weight of 2000.

[0052] Step 2: After the reaction in the first step is comple...

Embodiment 3

[0056] (a) Preparation of green and environmentally friendly silicon-based flame-retardant oligomers

[0057] Weigh 10g diphenylsilanediol (DPSD), 0.5g AlCl 3 and 50ml of toluene were fully dissolved in a three-necked flask. Stir under the conditions of 50° C. and 100 Pa, and react for 8 hours. After the reaction is complete, the product polyphenylsiloxane (PDPS) is obtained.

[0058] (b) Preparation of Nylon 6 Ester

[0059] Step 1: Add 100g of caprolactam, 4g of water, 2g of aminocaproic acid and 21.72g of adipic acid into the reaction kettle, pass nitrogen gas 3 times until the air in the kettle is replaced, and maintain a pressure of 0.05MPa, then raise the temperature to 240 ℃, stirred and reacted for 2 hours; the pressure in the kettle was adjusted to 300Pa, and the reaction was continued at 240℃ for 2 hours to obtain a carboxylated PA6 prepolymer with a molecular weight of 800.

[0060] Step 2: After the reaction in the first step is completed, adjust the pressure in...

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Abstract

The invention relates to a halogen-free molten-drop-resistant anti-flaming nylon-6 resin and a preparation method. The structural formula is as shown in the specification. The preparation method comprises the following steps: adding a nylon-6 esterification compound, polyphenyl siloxane PDPS, and an ester exchange catalyst to a reaction container, pumping nitrogen to displace the air in the container, reacting for 3-5 h in 160-200 DEG C of the temperature, regulating the pressure in the reaction container to be 0-200 Pa, and continuously reacting for 3-5 h, to obtain the halogen-free molten-drop-resistant anti-flaming nylon-6 resin. According to the preparation method, phenyl siloxane is introduced to the major structure of the nylon-6 in the chemical copolymerization mode, so a fire retardant is perfectly combined with the nylon-6. The mechanical property of the nylon-6 cannot be affected negatively, and the nylon-6 has the better and more lasting flame-retardant effect while the green and environmental property and the molten-drop-resistant property are endowed to the nylon-6.

Description

technical field [0001] The invention belongs to the field of flame retardant resin and its preparation, in particular to a halogen-free anti-droplet flame retardant nylon 6 resin and a preparation method thereof. Background technique [0002] Nylon 6 is a high-molecular material with fast burning speed and extremely high heat release. In addition, it will release a large amount of dense smoke accompanied by molten droplets during the burning process, which will cause serious damage to human body and ecological environment. At present, many researchers have done a lot of research work to improve the combustion performance of nylon 6, and it is gradually developing in the direction of environmental protection and good comprehensive performance. [0003] Patent CN 104311877A relates to a reactive nylon flame retardant and its preparation method, which is characterized in that: the halogen-free phosphorus-containing copolymerized flame retardant first reacts with glycol to obtai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/42C08G77/455C08G77/16C08G69/16C08G69/14
CPCC08G69/14C08G69/16C08G69/42C08G77/045C08G77/455C08G77/80
Inventor 李发学范硕吴德群王学利俞建勇
Owner DONGHUA UNIV
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