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Low permeability elastomeric-metal phosphate nanocomposites

a technology of elastomeric metal phosphate and nanocomposite composition, which is applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, chemical apparatus and processes, etc., can solve the problems of limited success, low reactivity and incompatibility with most, and difficult to disperse ionic nanofillers such as clay into generally inert, etc., to improve barrier and other desirable properties, improve performance, and improve the effect of exfoliation and/or

Active Publication Date: 2009-03-19
EXXONMOBIL CHEM PAT INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides elastomeric nanocomposites made with metal phosphate nanofillers dispersed in an isobutylene-based rubber, which have improved intercalation, exfoliation, and dispersion compared to previous nanofillers. The nanofiller is surface exchanged with an amine or amide-modified alpha-zirconium phosphate, which facilitates hydrogen bonding with the phosphate. The nanofiller can be intercalated, exfoliated, or a mixture of both. The resulting nanocomposite has improved barrier and other desirable properties.

Problems solved by technology

As a practical matter, it has thus proven to be very difficult to disperse ionic nanofillers such as clay into generally inert, nonpolar, hydrocarbon elastomers.
The prior art has, with limited success, attempted to improve dispersion by modification of the clay particles, by modification of the rubbery polymers, by the use of dispersion aids, and by the use of various blending processes.
The “inertness” of saturated hydrocarbon polymers such as BIMSM, their low reactivity and incompatibility with most other materials, and the difficulties in adhering them to, or using them in conjunction with most other materials has restricted their use in many areas.

Method used

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  • Low permeability elastomeric-metal phosphate nanocomposites
  • Low permeability elastomeric-metal phosphate nanocomposites
  • Low permeability elastomeric-metal phosphate nanocomposites

Examples

Experimental program
Comparison scheme
Effect test

case 1

[0265] 100 phr of BIMSM rubber was compounded with and without primary-primary diamine-treated zirconium phosphates (ZrP) and samples were tested for oxygen permeability. The BIMSM rubber (BIMSM A) had a para-methylstyrene (PMS) content of 10 wt %, and a benzylic bromine content of 0.85 mol % and a Mooney viscosity of about 32 (ML 1+8, 125° C., ASTM 1646. ZrP-HMDA-30-200 was a zirconium phosphate 30% exchanged with hexamethylene diamine with a platelet thickness of 6.3 {acute over (Å)}, length of 150-200 nm and aspect ratio greater than 250, and an aggregate particle thickness of 50 nm and length of 150-200 nm (approximately 40 layers per particle, surface area about 20 m2 / g), and ZrP-HMDA-30-400 was a similar zirconium phosphate 30% exchanged with a platelet thickness of 6.3 {acute over (Å)}, length of 150-400 nm and aspect ratio greater than 500, and an aggregate particle thickness of 20 nm and length of 150-400 nm (approximately 15 layers per particle, surface area about 35 m2 / g)...

case 2

[0268] 100 phr of a BIMSM rubber was compounded with and without a primary-tertiary diamine-treated zirconium phosphate (ZrP) and samples were tested for oxygen permeability. The BIMSM elastomer was BIMSM A as described above. ZrP-APM-100-400 was a zirconium phosphate 100% exchanged with N-3-aminopropyl-morpholine with a platelet aspect ratio of 150-400. N330 carbon black was added at 37 phr. The Zr—P was blended at 4 wt %, with an HSt / ZnO / MBTS curing system at 1 / 1 / 1 phr. The rubber was loaded into a Brabender® mixer at a temperature of 100-120° C. and mixed with the Zr—P and the carbon black for 7 minutes. The mixture was further mixed with the curatives package of equal parts by weight of stearic acid (HSt), zinc oxide (ZnO), and zinc dimethyl dithiocarbamate (ZDMDC), at 90° C. and 40 rpm for 3 minutes. The resulting rubber compounds were milled, compression molded and cured at 170° C. Pads were then prepared and tested as described above.

[0269]The permeability results are present...

example 3

[0270 demonstrates that the addition of the zirconium phosphate nanofiller according to the present invention reduced the permeability by 27% in this example.

[0271]Prophetic Examples 4-11: Cyclohexane (1.7 L) is added to a jacketed glass reactor and heated to 60° C. About 192 to 200 grams of BIMSM elastomer A (described above) are then added to the heated reactor. After all of the elastomer is completely dissolved, 16 grams of ZrP-APM-50-400 (a zirconium phosphate 50% exchanged with N-3-aminopropyl-morpholine with a platelet aspect ratio of about 50 to 400) and 4 or 8 grams of polyisobutylene succinic anhydride (PIBSA) in 50 mL of cyclohexane are added to the reactor and stirred for 40 minutes to form a cement. (The PIBSA is a polyisobutylene succinic anhydride having an Mw of 2,200 and about 2.5 mole % succinic anhydride.) The cement is then poured out and the solvent evaporated. The residual solid is dried under vacuum at 100° C. overnight to form a nanofiller-rubber mixture.

[0272...

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Abstract

The present invention provides a nanocomposite of an isobutylene-based elastomer and a phosphate nanofiller. Also disclosed is a nanocomposite embodiment wherein the elastomer is BIMSM and high aspect ratio, partially intercalated, partially exfoliated alpha-zirconium phosphate treated with amine or amide. A dispersion aid can include a low molecular weight polymer or oligomer, optionally functionalized with a polar group. The nanocomposite is suitable for use as an air barrier.

Description

FIELD OF THE INVENTION[0001]This invention relates to low permeability elastomeric-metal phosphate nanocomposite compositions, more particularly to isobutylene-based elastomers containing platy nano-fillers of alpha-zirconium phosphate, and especially to halogenated isobutylene elastomers, such as halogenated poly(isobutylene-co-p-methylstyrene) elastomers, particularly brominated poly(isobutylene-co-p-methylstyrene) elastomers (BIMSM), filled with alpha-zirconium phosphate exchanged with monoamines, diamines, tertiary amines, polyamides, or a combination thereof, with or without a dispersion aid such as low molecular weight polar modified polymer.BACKGROUND OF THE INVENTION[0002]Polymers with a saturated hydrocarbon backbone are well known to possess good environmental and aging resistance which makes them highly desirable in a variety of applications. In comparison with many other common elastomers, polyisobutylene and its copolymers are notable for their low permeability to small...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C08K3/32C08K3/10C08K5/17C08K5/20C08K5/00C08K5/098
CPCC08K9/04B82Y30/00C08K9/08C08K2201/008C08K2201/011C08L23/22
Inventor DE PUYDT, YVES FERNANDROBBERECHTS, HERMANTSOU, ANDY H.
Owner EXXONMOBIL CHEM PAT INC
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