Electrospinning of epoxy fibers

Patent metadata

Field	Value
Publication number	US-2023415378-A1
Application number	US-202218049648-A
Country	US
Kind code	A1
Filing date	Oct 26, 2022
Priority date	Jun 23, 2022
Publication date	Dec 28, 2023
Grant date	—

Abstract

The presently disclosed subject matter relates to the field of electrospun epoxy fibers, a solution for producing the fibers and a system for electrospinning the fibers. This invention further relates to processes of producing the solution and the fibers. By dissolving epoxy in a dielectric solvent, suitable electrospinning conditions are achieved by controlling the degree of epoxy crosslinking in the solution. The fibers are captured on a net screen, with the positive electrode placed behind it. The resulting electrospun fibers exhibit superior mechanical properties in comparison with other epoxy fibers. This improvement in mechanical properties is, in part, due to anisotropic molecular rearrangement resulting from the strong stretching forces induced by electrospinning.

First claim

1 . A method of producing an electrospinning epoxy solution, said method comprising:
mixing an epoxy resin with an epoxy hardener, producing an epoxy; adding a dielectric solvent to said epoxy, producing an epoxy solution; and stirring said epoxy solution to produce an electrospinning epoxy solution.

2 . The method of claim 1 wherein said epoxy resin is selected from a group comprising: bisphenol-based resins, novolaks-based resins, aliphatic-based resins, halogenated resins, glycidylamine-based resins or combinations thereof.

3 . The method of claim 1 wherein said dielectric solvent comprises methyl ethyl ketone (MEK), dimethylformamide (DMF), tetrahydrofuran (THF) or any combination thereof.

4 . The method of claim 1 wherein the weight fraction of said dielectric solvent ranges between 50%-99% of the total solution weight.

5 . The method of claim 1 wherein said stirring comprises a first stage and a second stage, wherein:
the stirring rate of said first stage is higher than the stirring rate of said second stage; or
the duration of stirring in said first stage is shorter than the duration of the stirring in said second stage; or

the temperature of said epoxy solution during said first stage is lower than the temperature of said epoxy solution during said second stage; or any combination thereof.

6 . The method of claim 5 wherein the stirring rate of said first stage ranges between 500 to 2000 rpm and the stirring rate of said second stage ranges between 100-500 rpm.

7 . The method of claim 5 wherein said duration of stirring in said first stage ranges between 1 minute to 1 hour and the said duration of stirring in said second stage ranges between 1 hour and 15 days.

8 . The method of claim 5 wherein said temperature during said first stage is about room temperature and wherein said temperature during said second stage ranges between 50-150° C.

9 . The method of claim 1 wherein said stirring stops when said epoxy solution reaches a state between pre-gelation and vitrification, producing an electrospinning epoxy solution.

10 . An electrospinning epoxy solution produced by the method of claim 1 .

11 . A system for electrospinning epoxy fibers, said system comprising:
a syringe barrel, said barrel being at least partially filled with the electrospinning epoxy solution of claim 10 ; an electrically grounded nozzle; a needle; a syringe pump for feeding said electrospinning epoxy solution out of said needle; a fiber collector; an electrode positioned behind said fiber collector; and a power supply; wherein said syringe pump is configured to eject said electrospinning epoxy solution from said needle when applying a voltage between said nozzle and said electrode, producing epoxy fibers which collect on said fiber collector.

12 . The system of claim 11 wherein the inner diameter of said needle ranges between 0.5 to 1 mm.

13 . The system of claim 11 wherein said fiber collector is made of a metal mesh.

14 . The system of claim 11 wherein the distance from said nozzle to said fiber collector ranges between 5 to 30 cm and the distance from said fiber collector to said electrode ranges between 0.5 to 5 cm.

15 . A method of producing epoxy fibers, said method comprising:
providing the system of claim 11 ; applying a voltage between said grounded nozzle and said electrode resulting in said electrospinning epoxy solution exiting through said nozzle producing an airborne jet which lands on said fiber collector producing epoxy fibers.

16 . The method of claim 15 wherein the feed rate of said electrospinning epoxy solution ranges between 0.1 to 10 ml/hr.

17 . The method of claim 15 wherein said applied voltage ranges between 1 to 30 kV.

18 . The method of claim 15 further comprising curing said epoxy fibers, said curing comprising:
leaving said epoxy fibers to rest for a duration of between 1 to 24 hrs after they are produced;
placing said epoxy fibers under vacuum for a duration of between 24 to 72 hrs;
placing said epoxy fibers in an oven at a temperature of between 50 to 200° C. for between 1 to 10 hrs;
or any combination thereof.

19 . An electrospun epoxy fiber produced by the method of claim 15 .

20 . An electrospun epoxy fiber comprising:
an epoxy resin; and an epoxy hardener;

21 . The electrospun epoxy fiber of claim 20 wherein the diameter of said electrospun epoxy fiber ranges between about 200 nm to 25 μm.

22 . The electrospun epoxy fiber of claim 20 wherein the length of said electrospun epoxy fiber ranges between 1 mm and 10 m.

23 . The electrospun epoxy fiber of claim 20 wherein the strength of said electrospun epoxy fiber ranges between 50 to 350 MPa.

24 . The electrospun epoxy fiber claim 20 wherein the maximum strain of said electrospun epoxy fiber ranges between 80 to 130%.

25 . The electrospun epoxy fiber of claim 20 wherein the Young's Modulus of said electrospun epoxy fiber ranges between 1000 to 3500 MPa.

26 . The electrospun epoxy fiber of claim 20 wherein the effective toughness of said electrospun epoxy fiber ranges between 25 to 200 MPa.

Assignees

• Yeda Res & Dev

Inventors

• Wagner Daniel Hanoch
• Shneider Mark

Classifications

• B29B7/005 Primary

  for mixing in batches · CPC title

• B29B7/10

  rotary · CPC title

• D01D5/003

  the material being a polymer solution or dispersion (D01D5/0053 takes precedence) · CPC title

• D04H1/4326 Primary

  Condensation or reaction polymers · CPC title

• D04H1/728

  by electro-spinning {(electro-spinning methods and apparatus D01D5/0007)} · CPC title