Polyamide composites containing graphene

Hye Jin Park

Patent

Atlas literature

Patent

US 9,469,742

Polyamide composites containing graphene

Hye Jin Park

Claims

Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.

21 independent · 23 dependent

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Independentgraphitic or graphenic materialgraphite oxidelactam monomernon-ionic surfactant
A method for producing polyamide composites containing graphene, comprising the following steps: (i) dispersing a graphitic or graphe nic material in an aqueous medium to yield an exfoliated material, and optionally removing non-reacted starting material from the aqueous mixture; (ii) mixing at least one lactam monomer with the aqueous mixture obtained in step (i); (iii) adding at least one non-ionic surfactant to the aqueous mixture obtained in step (ii); (iv) removing from the aqueous mixture obtained in step (iii) essentially all water contained therein; (v) heating the mixture obtained in step (iv) to 100 to 200 °C; (vi) if the water content of the mixture obtained in step (v) is higher than 300 ppm, subjecting the mixture obtained in step (v) to a further drying process to obtain a mixture with a water content of at most 300 ppm; (vii) heating the mixture obtained in step (v) or (vi) to 100 to 200 °C; (viii) adding an anionic polymerization activator; (ix) adding an anionic polymerization catalyst; and (x) after polymerization is completed, isolating the resulting polyamide composite; where the graphitic or graphenic material used in step (i) and the at least one non-ionic surfactant added in step (iii) are used in a weight ratio of from 20:1 to 1:1.
1. 22
  Dependent← claim 21graphite oxide
  The method as claimed in claim 21, where the graphitic or graphenic material used in step (i) is graphite oxide.
2. 23
  Dependent← claim 21
  The method as claimed in claim 21, where dispersing in step (i) is carried out by a sonication treatment, high speed mixing or high pressure homogenization.
3. 24
  Dependent← claim 21lactam monomer
  The method as claimed in claim 21, where the at least one lactam monomer used in step (ii) is selected from the group consisting of s -caprolactam, 2- piperidone, 2-pyrrolidone, caprylolactam, enantholactam, laurolactam and mixtures thereof.
4. 26
  Dependent← claim 21
  The method as claimed in claim 21, where the graphitic or graphenic material and the at least one lactam monomer are used in a weight ratio of from 1:5 to 1:5000.
5. 27
  Dependent← claim 21
  The method as claimed in claim 21, where the graphitic or graphenic material and the at least one lactam monomer are use in a weight ratio of from 1:10 to 1:1000.
6. 28
  Dependent← claim 21non-ionic surfactant
  The method as claimed in claim 21, where the at least one non-ionic surfactant used in step (iii) is selected f r om the group consisting of alcohols, alky l phenols, amines, amides, arylphenols, fatty acids or fatty acid esters alkoxylated with 1 to 100 equivalents of ethylene oxide and/or propylene oxide; and ethylene oxide/propylene oxide copolymers with a number average molecular weight M n of from 500 to 10000.
7. 30
  Dependent← claim 21
  The method as claimed in claim 21, where the graphitic or graphe nic material used in step (i) and the at least one non-ionic surfactant added in step (iii) are used in a weight ratio of from 20:1 to 1:1. 2, preferably from 5:1 to 1:1. 2, in particular from 3:1 to 1:1.
8. 31
  Dependent← claim 21
  The method as claimed in claim 21, where the graphitic or graphenic material used in step (i) and the at least one non-ionic surfactant added in step (iii) are used in a weight ratio of from 5:1 to 1:1.2.
9. 32
  Dependent← claim 21
  The method as claimed in claim 21, where the graphitic or graphenic material used in step (i) and the at least one non-ionic surfactant added in step (iii) are used in a weight ratio of from 3:1 to 1:1.
10. 33
  Dependent← claim 21
  The method as claimed in claim 21, where in step (v) the mixture is heated to 120 to 160 °C.
11. 34
  Dependent← claim 21
  The method as claimed in claim 21, where in step (vi) the mixture obtained in step (v) is subjected to a further drying process to obtain a mixture with a water content of at most 100 ppm.
12. 35
  Dependent← claim 21
  The method as claimed in claim 21, where in step (vii) the mixture is heated to 120 to 160 °C.
13. 36
  Dependent← claim 21
  The method as claimed in claim 21, where anionic polymerization activator added in step (viii) is selected from the group consisting of isocyanates, capped isocyanates, anhydrides, acyl halides, esters, ureas, allophanates and carbodiimides.
14. 40
  Dependent← claim 21
  The method as claimed in claim 21, where the anionic polymerization catalyst added in step (ix) is selected from the group consisting of sodium caprolactamate, potassium caprolactamate, magnesium bromide caprolactamate, magnesium chloride caprolactamate, magnesium biscaprolactamate, sodium hydride, sodium, sodium hydroxide, sodium methanolate, sodium ethanolate, sodium propanolate, sodium butanolate, potassium hydride, potassium, potassium hydroxide, potassium methanolate, potassium ethanolate, potassium propanolate, potassium butanolate and mixtures thereof.
15. 42
  Dependent← claim 21polyamide composite containing graphene
  Polyamide composite containing graphene, obtained by the method as claimed in claim 21.

Materials

Materials described outside the worked examples.

graphitic or graphenic material

Filler/Reinforcement Precursor

graphite oxide

Graphenic Precursor Material

Process steps

Additional fabrication and treatment steps described in the patent.

Anionic Polymerization

Step 1

Temperature

100, 200°C

Process details

steps:disperse graphitic/graphenic material in aqueous medium (sonication, high speed mixing, or high pressure homogenization), mix lactam monomer with aqueous dispersion, add non-ionic surfactant, remove essentially all water, heat to 100-200 C, optional further drying to ≤300 ppm water, heat to 100-200 C, add anionic polymerization activator, add anionic polymerization catalyst, isolate polyamide composite after polymerization

water content threshold ppm:

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
graphite peak indicating unexfoliated stacking	25–30 deg	graphene
Temperature	100–200 °C

Why these are connected

Related documents with shared materials, methods, properties, or citations.

Polyamide composites containing graphene | Matter42 Literature