IP Library Granted Patent US 8,178,030
Granted Patent B2
US 8,178,030 · App. 12/689,334 · Granted May 15, 2012

Electrospinning of PTFE with high viscosity materials

Assignee: Zeus Industrial Products, Inc.
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Quick Facts
Patent No.
US 8,178,030
App. No.
12/689,334
Granted
May 15, 2012
Kind
B2
Abstract

An improved process for forming a PTFE mat is described. The process includes providing a dispersion with PTFE, a fiberizing polymer and a solvent wherein said dispersion has a viscosity of at least 50,000 cP. An apparatus is provided which comprises a charge source and a target a distance from the charge source. A voltage source is provided which creates a first charge at the charge source and an opposing charge at the target. The dispersion is electrostatically charged by contact with the charge source. The electrostatically charged dispersion is collected on the target to form a mat precursor which is heated to remove the solvent and the fiberizing polymer thereby forming the PTFE mat.

Claims (59)

1. A process for forming a PTFE mat comprising:

providing a dispersion comprising:

PTFE;

a fiberizing polymer; and

a solvent wherein said dispersion has a viscosity of at least 50,000 cP;

providing an apparatus comprising a charge source and a target a distance from said charge source;

providing a voltage source to create a first charge at said charge source and an opposing charge at said target wherein said dispersion is electrostatically charged by contact with said charge source;

collecting said electrostatically charged dispersion on said target to form a mat precursor; and

heating said mat precursor to remove said solvent and said fiberizing polymer thereby forming said PTFE mat.

2. The process for forming a PTFE mat of claim 1 wherein said dispersion comprises 50-80 wt % PTFE solids.

3. The process for forming a PTFE mat of claim 2 wherein said dispersion comprises 59-61 wt % PTFE solids.

4. The process for forming a PTFE mat of claim 1 further comprising sintering.

5. The process for forming a PTFE mat of claim 4 wherein said sintering is at a temperature of at least 500° F. to no more than 900° F.

6. The process for forming a PTFE mat of claim 1 wherein said dispersion has a viscosity of at least 100,000 cP to no more than 300,000 cP.

7. The process for forming a PTFE mat of claim 1 comprising providing a voltage of 2,000 to 80,000 volts across said orifice and said target.

8. The process for forming a PTFE mat of claim 1 wherein said dispersion comprises at least 1 wt % to no more than 10 wt % of said fiberizing polymer.

9. The process for forming a PTFE mat of claim 1 wherein said dispersion comprises a weight ratio of fiberizing polymer to PTFE of at least 3.0 to no more than 5.5.

10. The process for forming a PTFE mat of claim 1 wherein said fiberizing polymer has a solubility in said solvent of greater than 0.5 wt %.

11. The process for forming a PTFE mat of claim 1 wherein said solvent is water.

12. The process for forming a PTFE mat of claim 1 wherein said fiberizing polymer has an ash content of less than 5 wt % upon sintering at 400° C.

13. The process for forming a PTFE mat of claim 1 wherein said fiberizing polymer is selected from the group consisting of dextran, alginates, chitosan, guar gum compounds, starch, polyvinylpyridine compounds, cellulosic compounds, cellulose ether, hydrolyzed polyacrylamides, polyacrylates, polycarboxylates, polyvinyl alcohol, polyethylene oxide, polyethylene glycol, polyethylene imine, polyvinylpyrrolidone, polyacrylic acid, poly(methacrylic acid), poly(itaconic acid), poly(2-hydroxyethyl acrylate), poly(2-(dimethylamino)ethyl methacrylate-co-acrylamide), poly(N-isopropylacrylamide), poly(2-acrylamido-2-methyl-1-propanesulfonic acid), poly(methoxyethylene), poly(vinyl alcohol), poly(vinyl alcohol) 12% acetyl, poly(2,4-dimethyl-6-triazinylethylene), poly(3-morpholinylethylene), poly(N-1,2,4-triazolyethylene), poly(vinyl sulfoxide), poly(vinyl amine), poly(N-vinyl pyrrolidone-co-vinyl acetate), poly(g-glutamic acid), poly(N-propanoyliminoethylene), poly(4-amino-sulfo-aniline), poly[N-(p-sulphophenyl)amino-3-hydroxymethyl-1,4-phenyleneimino-1,4-phenylene)], isopropyl cellulose, hydroxyethyl, hydroxylpropyl cellulose, cellulose acetate, cellulose nitrate, alginic ammonium salts, i-carrageenan, N-[(3′-hydroxy-2′,3′-dicarboxy)ethyl]chitosan, konjac glocomannan, pullulan, xanthan gum, poly(allyammonium chloride), poly(allyammonium phosphate), poly(diallydimethylammonium chloride), poly(benzyltrimethylammonium chloride), poly(dimethyldodecyl(2-acrylamidoethylyl) ammonium bromide), poly(4-N-butylpyridiniumethylene iodine), poly(2-N-methylpridiniummethylene iodine), poly(N methylpryidinium-2,5-diylethenylene), polyethylene glycol polymers and copolymers, cellulose ethyl ether, cellulose ethyl hydroxyethyl ether, cellulose methyl hydroxyethyl ether, poly(1-glycerol methacrylate), poly(2-ethyl-2-oxazoline), poly(2-hydroxyethyl methacrylate/methacrylic acid) 90:10, poly(2-hydroxypropyl methacrylate), poly(2-methacryloxyethyltrimethylammonium bromide), poly(2-vinyl-1-methylpyridinium bromide), poly(2-vinylpyridine N-oxide), poly(2-vinylpyridine), poly(3-chloro-2-hydroxypropyl-2-methacryloxyethyldimethylammonium chloride), poly(4-vinylpyridine N-oxide), poly(4-vinylpyridine), poly(acrylamide/2-methacryloxyethyltrimethylammonium bromide) 80:20, poly(acrylamide/acrylic acid), poly(allylamine hydrochloride), poly(butadiene/maleic acid), poly(diallyldimethylammonium chloride), poly(ethyl acrylate/acrylic acid), poly(ethylene glycol) bis(2-aminoethyl), poly(ethylene glycol) monomethyl ether, poly(ethylene glycol)-bisphenol A diglycidyl ether adduct, poly(ethylene oxide-b-propylene oxide), poly(ethylene/acrylic acid) 92:8, poly(1-lysine hydrobromide), poly(1-lysine hydrobromide), poly(maleic acid), poly(n-butyl acrylate/2-methacryloxyethyltrimethylammonium bromide), poly(N-iso-propylacrylamide), poly(N-vinylpyrrolidone/2-dimethylaminoethyl methacrylate), dimethyl sulfatequaternary, poly(N-vinylpyrrolidone/vinyl acetate), poly(oxyethylene) sorbitan monolaurate, poly(styrenesulfonic acid), poly(vinyl alcohol), N-methyl-4(4′-formylstyryl)pyridinium, methosulfate acetal, poly(vinyl methyl ether), poly(vinylamine) hydrochloride, poly(vinylphosphonic acid), poly(vinylsulfonic acid) sodium salt and polyaniline.

14. The process for forming a PTFE mat of claim 13 wherein said fiberizing polymer is polyethylene oxide.

15. The process for forming a PTFE mat of claim 14 wherein said polyethylene oxide has a molecular weight of at least 50,000 to no more than 4,000,000.

16. The process for forming a PTFE mat of claim 1 wherein said target is an expanded structure.

17. The process for forming a PTFE mat of claim 1 further comprising expanding or contracting said target.

18. The process for forming a PTFE mat of claim 1 further comprising expanding or contracting said target prior to said collecting.

19. A process for forming a PTFE mat comprising:

providing a dispersion comprising:

PTFE with a particle size of at least 0.1 microns to no more than 0.8 microns;

1 wt % to no more than 10 wt % of polyethylene oxide with a molecular weight of at least 50,000 to no more than 4,000,000; and

a solvent wherein said dispersion has a viscosity of at least 50,000 cP;

providing an apparatus comprising an orifice and a target a distance from said orifice;

providing a voltage source to create a first charge at said orifice and an opposing charge at said target;

forcing said dispersion through said orifice wherein said dispersion is electrostatically charged by contact with said orifice;

collecting said electrostatically charged dispersion on said target to form a mat precursor; and

heating said mat precursor to remove said solvent and said fiberizing polymer thereby forming said PTFE mat.

20. The process for forming a PTFE mat of claim 1 wherein said dispersion has a viscosity of at least 100,000 cP to no more than 500,000 cP.

21. The process for forming a PTFE mat of claim 6 wherein said viscosity is measured with a Brookfield LV Viscometer at a constant spindle speed setting of 2.5 for a #25 spindle at 25° C.

22. The process for forming a PTFE mat of claim 20 wherein said viscosity is measured with a Brookfield LV Viscometer at a constant spindle speed setting of 2.5 for a #25 spindle at 25° C.

23. A process for forming a PTFE mat comprising:

applying a voltage to establish an electrical charge differential between a charge source and a target;

electrostatically charging a dispersion, wherein the dispersion is electrostatically charged by the charge source, wherein the dispersion comprises PTFE, a fiberizing polymer, and a solvent, and wherein the dispersion has a viscosity of at least 50,000 cP;

collecting the electrostatically charged dispersion on the target, forming a mat precursor; and

heating the mat precursor to remove the solvent and the fiberizing polymer thereby forming the PTFE mat.

24. The process for forming a PTFE mat of claim 23 , wherein said dispersion has a viscosity of at least 100,000 cP to no more than 300,000 cP.

25. The process for forming a PTFE mat of claim 23 , wherein said dispersion has a viscosity of at least 100,000 cP to no more than 500,000 cP.

26. The process for forming a PTFE mat of claim 24 , wherein said viscosity is measured with a Brookfield LV Viscometer at a constant spindle speed setting of 2.5 for a #25 spindle at 25° C.

27. The process for forming a PTFE mat of claim 25 , wherein said viscosity is measured with a Brookfield LV Viscometer at a constant spindle speed setting of 2.5 for a #25 spindle at 25° C.

28. A process for forming a PTFE mat comprising:

applying a voltage to establish an electrical charge differential between a charge source and a target;

electrostatically charging a dispersion, wherein the dispersion is electrostatically charged by the charge source, wherein the dispersion comprises

PTFE with a particle size of at least 0.1 microns to no more than 0.8 microns,

1 wt % to no more than 10 wt % of polyethylene oxide with a molecular weight of at least 50,000 to no more than 4,000,000, and

a solvent,

wherein said dispersion has a viscosity of at least 50,000 cP;

collecting said electrostatically charged dispersion on said target, forming a mat precursor; and

heating said mat precursor to remove said solvent and said fiberizing polymer thereby forming said PTFE mat.

29. The process for forming a PTFE mat of claim 19 wherein said dispersion has a viscosity of at least 100,000 cP to no more than 300,000 cP, wherein said viscosity is measured with a Brookfield LV Viscometer at a constant spindle speed setting of 2.5 for a #25 spindle at 25° C.

30. The process for forming a PTFE mat of claim 19 wherein said dispersion has a viscosity of at least 100,000 cP to no more than 500,000 cP, wherein said viscosity is measured with a Brookfield LV Viscometer at a constant spindle speed setting of 2.5 for a #25 spindle at 25° C.

Assignments (5)
CHANGE OF NAME Recorded Apr 9, 2024
From: ZEUS COMPANY INC.
To: ZEUS COMPANY LLC
Reel/Frame 067043/0815 →
SECURITY INTEREST Recorded Feb 28, 2024
From: ZEUS COMPANY LLC
To: GOLDMAN SACHS BDC, INC., AS AGENT
Reel/Frame 066702/0187 →
CHANGE OF NAME Recorded Feb 27, 2024
From: ZEUS COMPANY INC.
To: ZEUS COMPANY LLC
Reel/Frame 066696/0788 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 25, 2022
From: ZEUS INDUSTRIAL PRODUCTS, INC.
To: ZEUS COMPANY INC.
Reel/Frame 058758/0410 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 19, 2010
From: ANNEAUX, BRUCE L.; BALLARD, ROBERT; GARNER, DAVID P.
To: ZEUS INDUSTRIAL PRODUCTS, INC.
Reel/Frame 023826/0353 →
Continuity (3)
Provisional Application 61145309 · Jan 16, 2009
Provisional Application 61256349 · Oct 30, 2009
Related Publication 20100193999A1 · Aug 5, 2010