HIGH-D E NSITY POLYET H YLENE-GRAP II ENE NANOCOMPOSITES AND

Mamdouh Ahmad AL-HARTHI

Patent

Atlas literature

Patent

US 10,150,850

HIGH-D E NSITY POLYET H YLENE-GRAP II ENE NANOCOMPOSITES AND

Mamdouh Ahmad AL-HARTHI

Drawings

Patent drawings and their descriptions. Click a drawing to enlarge it.

FIG. 1

FIG. 1. As can be seen from

FIG. 2

performance graph

FIG. 2 is a graph illustrating the heat release rates f o r polyethylene nan o composites measured via FAA m icrocalorimetry. DETA I LED DESCRIPTION OF THE …

Claims

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

7 independent · 13 dependent

2
Independent
Canceled
3
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the amount of the graphene nanosheets present during the polymerizing is 0.14-0.85 wt. % based on the total weight of the high-density polyethylene nanocomposite produced. Currently amended
4
Independent
Claims 4-6. Canceled
6
Independent
Canceled
7
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high- density polyethylene nanocomposite having a molecular weight of 30-120 kDa. Original
8
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high- density polyethylene nanocomposite having a polydispersity index of 3-12. Original
9
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high- density polyethylene nanocomposite that is non-ﬂammable. Original
10
Independent
Claims 10-15. Canceled
15
Independent
Canceled
16
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite, having a molecular weight of 30-120 kDa, a unimodal molecular weight distribution and a polydispersity index of 3-12. Previously presented
17
Independent
Canceled
18
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite having a total heat release of less than 33.34 kJ/kg. Previously presented
19
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite having a peak heat release rate of from 788.90 to 665.28 W/g. Previously presented
20
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite having a peak heat release rate of 665.28- 788. 9 W/g, a total heat release of 29.18-33.34 kJ/kg and a peak decomposition temperature of from 496.02 to 499.61 °C. Previously presented
21
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite having a weight average molecular weight of from 31,513.5 to 119,862.75 Da. Previously presented
22
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite having a crystalline melting temperature of from 132.47 to 132.72 °C. Previously presented
23
Dependent← claim 1high-density polyethylene nanocompositeC
The method of claim 1, wherein the polymerizing forms a high-density polyethylene nanocomposite comprising graphene in an amount of 0.14- 0.41 wt % and wherein said graphene nanoﬁller has a single layer thickness of 0.30-0.34 nm. Previously presented
24
Independent
Canceled
25
Dependent← claim 1high-density polyethylene nanocompositeCzirconoceneC₇H₈C₂H₄
The method of claim 1, wherein the second mixture consists of the toluene solvent, the zirconocene catalyst, the graphene nanosheets and the ethylene. New
1. 26
  Dependent← claim 25high-density polyethylene nanocompositeCzirconoceneC₇H₈C₂H₄methylaluminoxane (MAO)
  The method of claim 25, wherein the polymerization mixture consists of the toluene solvent, the zirconocene catalyst, the graphene nanosheets, the ethylene, and the methylaluminoxane co-catalyst. New

Worked examples

Embodiments described in the patent, grouped by the materials and process steps they use.

Example 1

example section example

5 materials

Materials sourcing: zirconocene catalyst, toluene solvent, methylaluminoxane (MAO) co-catalyst obtained from Aldrich Chemicals; graphene (96-99% purity, 50-100 nm) purchased from Grafen Chemical Industries Co (Turkey). All manipulations carried out under N₂ environment with Schlenk flask and glove box.

Example 2

example section example

6 materials1 process step

Synthesis of polyethylene nanocomposites via in situ polymerization. Ethylene polymerization in 250 mL round bottom flask with magnetic stirrer. Catalyst (6 mg), solvent (80 mL toluene) and graphene (5, 10, 15 or 30 mg) added inside glove box. Reactor immersed at 40°C constant temperature bath; nitrogen removed by vacuum pump and ethylene introduced. Co-catalyst added after ethylene saturation. Reaction time 30 min at 1000 rpm and 1.3 bar. Quenched with acidified methanol (5 vol.% HCl), filtered, washed with methanol, dried at 50°C. Graphene loadings: 5, 10, 15 mg = 0.14, 0.25, 0.41 wt.% (G₁/HDPE, G₂/HDPE, G₃/HDPE).

Example 3

example section example

2 materials

Characterization of G₁/HDPE, G₂/HDPE, G₃/HDPE nanocomposites and HDPE control. Average molecular weight by HT-GPC (triple detection, 25 mg in 10 mL 1,2,4-trichlorobenzene, 160°C). DSC on DSC-Q1000: heated to 160°C at 10°C/min, cooled to 30°C at 10°C/min under N2, second heating cycle used. Flammability by FAA microcalorimeter at 1°C/min to 900°C. Results: HDPE control Mw=30044.75 Da, PDI=4.13, Tm=131.86°C; G₁/HDPE Mw=31513.50 Da, PDI=3.17, Tm=132.72°C; G₂/HDPE Mw=119862.75 Da, PDI=11.55, Tm=132.47°C; G₃/HDPE Mw=78140.50 Da, PDI=8.17, Tm=132.61°C. FAA: G₁/HDPE peak HRR=665.28 W/g, total HR=29.18 kJ/kg, Tp=496.02°C.

Characterization

Measurements and analyses referenced in the patent, with their drawing references.

device performance measurement

Device Performance Measurement

FIG. 2 is a graph illustrating the heat release rates f o r polyethylene nan o composites measured via FAA m icrocalorimetry. DETA I LED DESCRIPTION OF THE …

Figure references

FIG. 2

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
Mw of HDPE control	30044.75 Da	high-density polyethylene nanocomposite
Mw of G1/HDPE (0.14 wt% graphene)

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