Process for making a nanocomposite and a polyethylene nanocomposite made therefrom

Patent metadata

Field	Value
Publication number	US-10294353-B2
Application number	US-201816130373-A
Country	US
Kind code	B2
Filing date	Sep 13, 2018
Priority date	Jul 10, 2015
Publication date	May 21, 2019
Grant date	May 21, 2019

Abstract

Methods of preparing high-density polyethylene (HDPE) nanocomposites by in situ polymerization with a zirconocene catalyst, a methylaluminoxane cocatalyst, a calcium zirconate nanofiller in a solvent. The calcium zirconate nanofiller, which is dispersed across the polyethylene matrix, is found to enhance catalyst activity, and other properties of the HDPE nanocomposites produced, including but not limited to flame retardency, crystallinity and surface morphology.

First claim

The invention claimed is:

1. A method for forming a high-density polyethylene nanocomposite by polymerizing a mixture of ethylene and a calcium zirconate nanofiller, comprising:
adding a zirconocene catalyst, the calcium zirconate nanofiller and a solvent to a reactor;
mixing the zirconocene catalyst and the calcium zirconate nanofiller in the solvent;
injecting ethylene into the reactor until absorption of ethylene is no longer observed; followed by
adding a methylaluminoxane cocatalyst into the reactor to from a catalyst mixture; then
polymerizing the ethylene by pressurizing the reactor with ethylene and maintaining a pressure of 1-1.5 bar to form a polymerization mixture; and then
quenching the polymerization mixture with methanol to form the high-density polyethylene nanocomposite;
wherein the calcium zirconate nanofiller is dispersed in a polyethylene matrix of the high-density polyethylene nanocomposite, and the polyethylene matrix has a melting temperature of 132.3 to 134.0° C. determined by DSC,
wherein the calcium zirconate nanofiller is not a support material for the zirconocene catalyst.

2. The method of claim 1 , wherein the calcium zirconate nanofiller is present in an amount of from 0.02 to 3.0 wt. % per total weight of the high-density polyethylene nanocomposite produced.

3. The method of claim 1 , wherein the solvent is toluene.

4. The method of claim 3 , wherein the zirconocene catalyst has a concentration of from 10 to 30 μmol in toluene.

5. The method of claim 3 , wherein the methylaluminoxane cocatalyst is present at a methylaluminoxane/toluene volume ratio of from 1:10 to 1:20.

6. The method of claim 1 , wherein the polymerizing is carried out at a temperature of from 25 to 35° C.

7. The method of claim 1 , wherein the average particle size of the calcium zirconate nanofiller is from 30 to 75 nm.

8. The method of claim 1 , wherein the calcium zirconate nanofiller increases the activity of the zirconocene catalyst by 5 to 45%.

9. The method of claim 1 , wherein the polymerizing forms a high-density polyethylene nanocomposite having 60 to 80% crystallinity.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Al-Harthi Mamdouh Ahmed

Classifications

• C08K3/24

  Acids; Salts thereof {(C08K3/16 takes precedence)} · CPC title

• G01K17/04

  Calorimeters using compensation methods {, i.e. where the absorbed or released quantity of heat to be measured is compensated by a measured quantity of heating or cooling} · CPC title

• C08K3/08

  Metals · CPC title

• G01N2030/486

  Physics · mapped topic

• C08L23/08

  Copolymers of ethene (C08L23/16 takes precedence) · CPC title