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Preparation method for graphene/nylon 6 nano composite material

A nanocomposite material and graphene technology, which is applied in the field of preparation of graphene/nylon 6 nanocomposite materials, can solve the problems of unfavorable large-scale preparation of graphene/nylon 6, increase in molecular weight, difficulty in polymerization, etc., and achieve large lateral size , comprehensive performance improvement, and the effect of improving compatibility

Inactive Publication Date: 2017-12-26
HANGZHOU GAOXI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In addition, the methods reported so far for the preparation of graphene / nylon 6 composites by in situ polymerization of graphene oxide dispersion and caprolactam are all based on the preparation process of batch reactors, and the polymerization system contains a large amount of water.
In the industry, most production lines of nylon 6 use VK tubes for continuous polymerization, which has high requirements on the water content of the polymerization system. Too much water content seriously inhibits the increase of molecular weight, and even makes it difficult to polymerize. This is a problem for graphene / nylon 6 large-scale preparation and its disadvantages

Method used

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  • Preparation method for graphene/nylon 6 nano composite material
  • Preparation method for graphene/nylon 6 nano composite material
  • Preparation method for graphene/nylon 6 nano composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Dry the single-layer graphene oxide dispersion by atomization drying method to obtain pleated spherical graphene oxide. Oxygen ratio is 5, water content is less than 0.1%;

[0023] (2) Add 3.5 parts by mass of pleated spherical graphene oxide and 2 parts by mass of deionized water into 100 parts by mass of caprolactam melt, and stir and mix at a high speed (400 rpm) at 80° C. to form a dispersion;

[0024] (3) Under the protection of nitrogen, add the above dispersion into the polycondensation reactor, and raise the temperature to 250-270°C, and react at 0.5-1MPa for 3 hours; then react under vacuum for 4 hours to obtain a polymer melt; finally The polymer melt is water-cooled and granulated to obtain a graphene / nylon 6 nanocomposite material.

[0025] Using this material for high-speed spinning, such as Figure 4 Silk rolls shown. Due to the high amount of graphene added, the silk is highly UV resistant and has an extremely low percolation threshold.

[0026] T...

Embodiment 2

[0028] (1) drying the single-layer graphene oxide dispersion by the atomization drying method to obtain pleated spherical graphene oxide, the atomization temperature is 130°C, the size of the graphene oxide sheet is 1 to 20 microns, and the average size is 10 microns, The carbon-oxygen ratio is 4.2, and the moisture content is less than 0.1%;

[0029] (2) Add 2 parts by mass of pleated spherical graphene oxide and 2 parts by mass of deionized water into 100 parts by mass of caprolactam melt, and stir and mix at a high speed (400 rpm) at 80° C. to form a dispersion;

[0030] (3) Under the protection of nitrogen, add the above dispersion into the polycondensation reactor, and raise the temperature to 250-270°C, and react at 0.5-1MPa for 3 hours; then react under vacuum for 4 hours to obtain a polymer melt; finally The polymer melt is water-cooled and granulated to obtain a graphene / nylon 6 nanocomposite material.

[0031] The performance of gained graphene / nylon 6 nanocomposite...

Embodiment 3

[0033] (1) drying the single-layer graphene oxide dispersion by atomization drying method to obtain pleated spherical graphene oxide, the atomization temperature is 130°C, the size of the graphene oxide sheet is 1 to 40 microns, and the average size is 20 microns, The carbon-oxygen ratio is 3.9, and the moisture content is less than 0.1%;

[0034] (2) Add 0.5 parts by mass of pleated spherical graphene oxide and 2 parts by mass of deionized water to 100 parts by mass of caprolactam melt, stir and mix at 80°C at high speed (400rpm) to form a dispersion;

[0035] (3) Under the protection of nitrogen, add the above dispersion into the polycondensation reactor, and raise the temperature to 250-270°C, and react at 0.5-1MPa for 3 hours; then react under vacuum for 4 hours to obtain a polymer melt; finally The polymer melt is water-cooled and granulated to obtain a graphene / nylon 6 nanocomposite material.

[0036] The performance of gained graphene / nylon 6 nanocomposite material is ...

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Abstract

The invention relates to a preparation method for a graphene / nylon 6 nano composite material. The graphene / nylon 6 composite material is obtained by performing in-situ polymerization on pleated-sphere-shaped oxidized graphene and caprolactam. In ring opening condensation polymerization period of a caprolactam monomer, the pleated-sphere-shaped oxidized graphene is gradually dissociated into single-layer oxidized graphene sheets, the single-layer oxidized graphene sheets are reacted with nylon 6 molecules to form covalent grafting, and at the same time thermal reduction is performed on the oxidized graphene. According to the invention, just a small number of the pleated-sphere-shaped oxidized graphene is added, thus mechanical properties, high-temperature resistance and ultraviolet aging resistance of nylon 6 can be remarkably improved, dispersity of the graphene in a polymer substrate is excellent, a usage amount is less, the final product has good machinability, and industrialized multi-tow high-speed spinning can be performed; and besides, the preparation process related by the invention is simple and effective, and suitable for industrialized VK tube polymerization equipment, modification of nylon 6 polymerization equipment does not need, and therefore the preparation method provided by the invention is a production technology which extremely has market competitiveness.

Description

technical field [0001] The invention belongs to the field of nylon composite materials, and in particular relates to a method for preparing a graphene / nylon 6 nanocomposite material with low graphene addition by using an in-situ polymerization method. Background technique [0002] Graphene is a two-dimensional single-layer layered material composed of carbon atoms. Graphene itself has high strength (130GPa), high thermal conductivity (5000W m ‐1 K ‐1 ), high conductivity (10 8 S m ‐1 ) and good gas barrier properties, it is an ideal layered nanofiller. Nylon 6 (polyamide 6) is the largest and most widely used product among nylon engineering plastics. It has good comprehensive performance and high cost performance. It can be used in many fields such as automobile industry, electric appliance industry, machinery industry, textile industry and civil living materials. [0003] Therefore, the nylon nanocomposite obtained by uniformly dispersing graphene in the nylon 6 syste...

Claims

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Application Information

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IPC IPC(8): C08G69/16C08K3/04C08L77/02
CPCC08G69/16C08K3/04C08L2201/08C08L2203/12C08L77/02
Inventor 高超陈琛韩燚
Owner HANGZHOU GAOXI TECH CO LTD
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