Nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers and preparation method thereof

A polylactic acid fiber, copolymerized flame-retardant technology, applied in the field of preparation of phosphorus-nitrogen synergistic copolymerized flame-retardant polylactic acid fiber, can solve the problems of poor mechanical properties of fibers, PLA easy to burn, poor compatibility, etc., and achieve excellent flame retardancy Performance and mechanical properties, short preparation process, and broad market prospects

Active Publication Date: 2016-05-25
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method is simple. On the one hand, it solves the problems of poor fiber mechanical properties and difficulty in fiber formation caused by the poor compatibility between the existing flame retardants and PLA;

Method used

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  • Nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of nitrogen-phosphorus synergistic copolymerization flame-retardant polylactic acid fiber, the specific steps are:

[0029] (1) Preparation of nitrogen-phosphorus synergistic flame retardant monomer (FR): with N 2 As protective gas, dissolve 0.1mol aminophenol (DDS) and 0.1mol p-hydroxybenzaldehyde (HBH) in 100ml solvent methanol, heat up to 40°C, and react for 4 hours to obtain the intermediate without separation and purification; 2 As a protective gas, take 0.1mol intermediate and 0.2mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and dissolve in 200ml tetrahydrofuran (THF), heat up to 40°C, After 10 hours of reaction, nitrogen-phosphorus synergistic flame retardant monomer (FR) can be obtained without separation and purification.

[0030] (2) Dry LA and FR at 80°C for 24 hours to remove moisture; dry the reaction vessel at 100°C for 1 hour to remove moisture, and continuously pass inert gas N 2 replace the air;

[0031] (3) FR an...

Embodiment 2

[0035] A preparation method of nitrogen-phosphorus synergistic copolymerization flame-retardant polylactic acid fiber, the specific steps are:

[0036] (1) Preparation of nitrogen-phosphorus synergistic flame retardant monomer (FR): with N 2 As a protective gas, dissolve 0.4mol aminophenol (DDS) and 0.4mol p-hydroxybenzaldehyde (HBH) in 300ml solvent methanol, heat up to 80°C, and react for 8 hours to obtain the intermediate without separation and purification; 2 As a protective gas, take 0.4mol of intermediates and 0.8mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and dissolve it in 800ml of tetrahydrofuran (THF), and heat up to 80°C , after 16 hours of reaction, the nitrogen-phosphorus synergistic flame retardant monomer (FR) can be obtained without separation and purification.

[0037] (2) Dry LA and FR at 80°C for 24 hours to remove moisture; dry the reaction vessel at 100°C for 1 hour to remove moisture, and continuously pass inert gas N 2 replace the ...

Embodiment 3

[0042] A preparation method of nitrogen-phosphorus synergistic copolymerization flame-retardant polylactic acid fiber, the specific steps are:

[0043] (1) Preparation of nitrogen-phosphorus synergistic flame retardant monomer (FR): with N 2 As a protective gas, dissolve 0.2mol aminophenol (DDS) and 0.2mol p-hydroxybenzaldehyde (HBH) in 200ml solvent methanol, heat up to 60°C, and react for 6 hours to obtain the intermediate without separation and purification; 2 As a protective gas, take 0.2mol of intermediate and 0.4mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and dissolve it in 500ml of tetrahydrofuran (THF), and heat up to 60°C , after 12 hours of reaction, the nitrogen-phosphorus synergistic flame retardant monomer FR can be obtained without separation and purification.

[0044] (2) Dry LA and FR at 80°C for 24 hours to remove moisture; dry the reaction vessel at 100°C for 1 hour to remove moisture, and continuously pass inert gas N 2 replace the air...

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Abstract

The invention provides nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers and a preparation method thereof. The preparation method of the nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers is characterized by comprising the steps that 1, a nitrogen-phosphorus synergetic flame retardant monomer (FR) is prepared; 2, under a vacuum or inert atmosphere, Sn(Oct)2 serves as a catalyst, the nitrogen-phosphorus synergetic flame retardant monomer (FR) and lactide (LA) are subjected to a ring opening copolymerization reaction at the temperature of 130-170 DEG C, and nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid (FR-PLA) is obtained; 3, nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid is subjected to vacuum drying, the moisture content of the nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid is made to be smaller than or equal to 80 ppm, melt spinning forming is conducted at the temperature of 200-240 DEG C, and the nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers are obtained. According to the nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers and the preparation method thereof, a copolymerization method is adopted to prepare the flame retardant PLA, the problems that compatibility between fire retardant and a base body is poor, the fire retardant is migrated and precipitated, and thermal stability in multiple times of melting machining is poor are effectively avoided, and the obtained flame retardant PLA has excellent spinnability and mechanical properties simultaneously.

Description

technical field [0001] The invention belongs to the field of functional modification of polylactic acid fiber products, in particular to a preparation method of phosphorus-nitrogen synergistic copolymerization flame-retardant polylactic acid fiber. Background technique [0002] Polylactic acid (PLA) is a linear aliphatic polyester based on plant starch, which is considered to be the most One of the promising bio-based degradable materials. However, PLA, like general-purpose polymer materials, has the problems of flammability and serious droplet, which limits the application of PLA in fields with high requirements for flame retardancy, such as automotive interiors and electronic packaging. At present, the flame retardant modification of PLA mainly adopts physical blending modification. The national invention patent CN10831156A discloses a halogen-free toughened flame retardant PLA blend material, in which the amount of flame retardant added is as high as 5-30wt%; the nationa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/84C08G18/73C08G18/66C08G18/42C08G63/08
CPCC08G18/428C08G18/6633C08G18/73C08G63/08D01F6/84
Inventor 朱美芳俞森龙相恒学周家良左伟伟
Owner DONGHUA UNIV
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