A high-performance monomer casting nylon/graphene nanocomposite material and its in-situ polymerization preparation method

A nanocomposite material and technology of composite material, applied in the field of monomer casting nylon/graphene nanocomposite material and its preparation, can solve the problems of strong van der Waals force, unfavorable graphene dispersibility and compatibility, easy agglomeration, etc. Improve mechanical properties and enhance the effect of interfacial intercalation

Active Publication Date: 2017-07-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN 101928457 A discloses a cast nylon / graphene composite material directly added with 0.1-5% graphene in situ polymerization, the mechanical properties of the prepared composite material are improved, but the impact resistance and friction performance are relatively low Difference
The addition of graphene makes MC nylon have excellent mechanical, thermal, electrical and other comprehensive properties. However, in the above preparation methods, directly incorporating graphene into the matrix is ​​not conducive to the dispersion and compatibility of graphene in the MC nylon matrix. Or the graphene coupling modification method is relatively cumbersome
Graphene with a complete structure is composed of benzene rings, with high chemical stability, inert surface, and weak interaction with other media; and there is strong van der Waals force between graphene sheets, which is easy to agglomerate, which greatly limits its research and application; how to use efficient A simple and easy-to-implement method to achieve good dispersion of graphene in nylon matrix is ​​the key to the preparation of high-performance MC nylon / graphene nanocomposites

Method used

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  • A high-performance monomer casting nylon/graphene nanocomposite material and its in-situ polymerization preparation method
  • A high-performance monomer casting nylon/graphene nanocomposite material and its in-situ polymerization preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Disperse 1g of graphene oxide in 1000g of ethanol / water mixture with a volume ratio of 1 / 1, add 3g of hydroxy-terminated polyethylene oxide with a molecular weight of 400g / mol, stir uniformly at room temperature, and use ultraviolet light to coordinate ultrasonic dispersion for 30 minutes. The wavelength is 200nm, the power is 600W, the ultrasonic power is 500W, the frequency is 20000Hz, the ultrasonic temperature is 80℃; then 2g of hydrazine hydrate is added, and the reaction is reduced in 80℃ oil bath for 10h. The product is filtered and washed with distilled water at 90℃ Dry for 8h to constant weight;

[0021] Fully melt 100g of caprolactam at 105°C, add 1g of graphene oxide that has been coupled and reduced, and disperse for 20min under ultrasound with a power of 600W and a frequency of 10000Hz; then heat to 130°C, and distill under reduced pressure to remove water; Then add 0.20g of sodium hydroxide into the reaction kettle, perform vacuum distillation again to remove...

Embodiment 2

[0023] Disperse 5g of graphene oxide in 10000g of ethanol / water mixture with a volume ratio of 1 / 1, add 10g of hydroxy-terminated polyoxypropylene with a molecular weight of 2000g / mol, stir uniformly at room temperature, and use ultraviolet light to coordinate ultrasonic dispersion for 100 minutes. The wavelength is 400nm, the power is 400W, the ultrasonic power is 1000W, the frequency is 40000Hz, the ultrasonic temperature is 60℃; then 10g sodium borohydride is added, and the reaction is reduced in an oil bath at 100℃ for 6h. The product is filtered and washed with distilled water at 90 Dry for 8h at ℃ to constant weight;

[0024] Fully melt 100g caprolactam at 110°C, add the above-mentioned coupled and reduced graphene oxide 5g, disperse for 30min under ultrasound with a power of 2000W and a frequency of 30000Hz; then heat up to 140°C, and distill under reduced pressure to remove water; Then add 0.50g of sodium methoxide into the reaction kettle, perform vacuum distillation aga...

Embodiment 3

[0026] Disperse 2g of graphene oxide in 4000g of ethanol / water mixture with a volume ratio of 1 / 1, add 2g of amino-terminated polyoxypropylene ether with a molecular weight of 10000g / mol, stir uniformly at room temperature, and use microwave to coordinate ultrasonic dispersion for 200min, microwave frequency It is 200MHz, power is 1000W, ultrasonic power is 800W, frequency is 60000Hz, ultrasonic temperature is 50℃; then add 20g vitamin C, reduce reaction in 60℃ oil bath for 4h, product is filtered, washed with distilled water, dried at 90℃ for 8h To constant weight

[0027] Fully melt 100g caprolactam at 120°C, add the above-mentioned 0.7g graphene oxide after coupling and reduction treatment, and disperse for 50min under ultrasound with power of 100W and frequency 50000Hz; then heat to 150°C, and distill under reduced pressure to remove water ; Then 1g of sodium caprolactam was added to the reactor, vacuum distillation was performed again to remove water, the temperature was rai...

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Abstract

The invention discloses a high-performance monomer casting nylon / graphene nanometer composite material and an in-situ polymerization preparation method of the high-performance monomer casting nylon / graphene nanometer composite material. The preparation method is characterized in that 100 parts of caprolactam are completely melted at 90 DEG C to 130 DEG C; 0.1 to 20 parts of graphene oxide subjected to coupling and reduction treatment are added; the dispersion is performed for 10 to 100 minutes under the effect of ultrasound with the powder being 100 to 3000w and the frequency being 10000 to 100000HZ; the temperature is raised to 125 DEG C to 150 DEG C, and reduced pressure distillation is performed to remove water; then, 0.01 to 10 parts of base catalysts are added into a reaction kettle; vacuum distillation is performed for removing water again; the temperature is raised to 135 to 160 DEG C; vacuum is released; 0.01 to 10 parts of polyisocyanate activating agents are fast added; the mixture is uniformly stirred and is fast injected into a mold preheated to 160 to 200 DEG C; the polymerization reaction is performed for 20 to 120 minutes; the demolding is performed after natural cooling.

Description

Technical field [0001] The invention relates to a monomer cast nylon / graphene nano composite material and a preparation method thereof, and belongs to the field of polymer synthesis and processing. Background technique [0002] Monomer cast nylon (MC nylon for short) is a new type of engineering plastic developed by the application of caprolactam anionic ring-opening polymerization technology. It has high molecular weight, high crystallinity, and high density. Therefore, its mechanical strength, stiffness and wear resistance are better than ordinary nylon. It has good chemical properties, low water absorption, good dimensional stability, and can adopt a bulk polymerization method that combines polymerization and molding in a hot mold. It is especially suitable for large nylon molded products. It is gradually replacing copper and aluminum in many fields. , Steel and other metal materials, widely used in machinery, petrochemical, textile, transportation, construction, metallurgy an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/14C08G69/20C08K9/04C08K3/04
Inventor 叶林向萌李成杰
Owner SICHUAN UNIV
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