Identification of π-interactions of mesophase formation, and methods related thereto

Patent metadata

Field	Value
Publication number	US-12455239-B2
Application number	US-202217816526-A
Country	US
Kind code	B2
Filing date	Aug 1, 2022
Priority date	Aug 1, 2022
Publication date	Oct 28, 2025
Grant date	Oct 28, 2025

Abstract

Identification of aromatic interactions, e.g. π-interactions, of mesophase formation, and methods related thereto, including the use of fluorescent light and optical imaging and/or detection schemes for the identification of π-interactions of mesophase formation, and methods related thereto. Methods include interacting fluorescent light with a pitch composition; receiving fluorescent light emissions from the pitch composition; and detecting the onset of mesophase formation upon detecting a normalized fluorescence intensity (I/I 0 ) of the fluorescent light emissions in the range of about 0.4 to about 0.7 at a wavelength in the range of about 430 nm to about 470 nm for an exposure of about 1.5 seconds.

First claim

What is claimed is:

1. A method comprising:
interacting fluorescent light with a pitch composition;
receiving fluorescence emissions from the pitch composition;
acquiring a fluorescent light image via a band-pass excitation filter and a long-pass emission filter of the received fluorescence emissions;
identifying spatial variations in the fluorescent light images, wherein the spatial variations are a measure of change in a hydrogen to carbon ratio as measured according to ASTM D5291; and
identifying mesophase region and isotropic region in the pitch composition by quantitatively characterizing variations in composition based at least in part on the hydrogen to carbon ratio.

2. The method of claim 1 , wherein the interacting fluorescent light with a pitch composition is performed in real time or periodically as the pitch composition is pyrolyzing.

3. The method of claim 2 , wherein the pyrolyzing is performed at a temperature in the range of about 300° C. to about 600° C.

4. The method of claim 2 , wherein the pyrolyzing is performed during carbon fiber production.

5. The method of claim 2 , further comprising ceasing the pyrolyzing upon detecting the onset of mesophase formation.

6. The method of claim 2 , wherein the interacting fluorescent light with a pitch composition is performed in real-time as the pitch composition is pyrolyzing, and further comprising continuing the pyrolyzing until the H/C Ratio is in the range of about 0.5 to about 1.05.

7. The method of claim 2 , wherein the interacting fluorescent light with a pitch composition is performed in real-time as the pitch composition is pyrolyzing, and further comprising continuing the pyrolyzing until the I/I 0 is in the range of about 0.4 to about 0.7 at a wavelength in the range of about 430 nm to about 470 nm for an exposure of about 1.5 seconds, and the H/C Ratio is in the range of about 0.5 to about 1.05.

8. The method of claim 1 , wherein the interacting fluorescent light has a wavelength in the range of about 10 nanometers (nm) to about 1400 nm.

9. The method of claim 8 , wherein the interacting fluorescent light has a wavelength in the range of about 700 nm to about 1400 nm.

10. A method comprising:
interacting fluorescent light with a pitch composition;
receiving fluorescence emissions from the pitch composition;
acquiring a fluorescent light image via a band-pass excitation filter and a long-pass emission filter of the received fluorescence emissions;
subjecting the fluorescent light image to digital contrast enhancement;
identifying spatial variations in the fluorescent light images, wherein the spatial variations are a measure of change in a hydrogen to carbon ratio as measured according to ASTM D5291; and
identifying mesophase region and isotropic region in the pitch composition by quantitatively characterizing variations in composition based at least in part on the hydrogen to carbon ratio.

11. The method of claim 10 , wherein the interacting fluorescent light with a pitch composition is performed in real time or periodically as the pitch composition is pyrolyzing.

12. The method of claim 11 , wherein the pyrolyzing is performed at a temperature in the range of about 300° C. to about 600° C.

13. The method of claim 11 , wherein the pyrolyzing is performed during carbon fiber production.

14. The method of claim 11 , further comprising ceasing the pyrolyzing upon detecting the onset of mesophase formation.

15. The method of claim 10 , wherein the interacting fluorescent light with a pitch composition is performed in real-time as the pitch composition is pyrolyzing, and further comprising continuing the pyrolyzing until the H/C Ratio is in the range of about 0.5 to about 1.05.

16. The method of claim 10 , wherein the interacting fluorescent light with a pitch composition is performed in real-time as the pitch composition is pyrolyzing, and further comprising continuing the pyrolyzing until normalized fluorescent intensity (I/I 0 ) is in the range of about 0.4 to about 0.7 at a wavelength in the range of about 430 nm to about 470 nm for an exposure of about 1.5 seconds, and the hydrogen to carbon ratio (H/C Ratio) is in the range of about 0.5 to about 1.05.

17. The method of claim 10 , wherein the onset of mesophase formation correlates to the generation of π-interactions.

18. A method comprising:
interacting fluorescent light with a pitch composition;
capturing fluorescence emissions from the pitch composition;
acquiring a fluorescent light image from the captured fluorescence emissions;
identifying spatial variations in the fluorescent light images, wherein the spatial variations are a measure of change in a hydrogen to carbon ratio as measured according to ASTM D5291; and
identifying mesophase region and isotropic region in the pitch composition by quantitatively characterizing variations in composition based at least in part on the hydrogen to carbon ratio.

Assignees

• Exxonmobil Technology & Engineering Company
• Exxon Mobil Tech And Engineering Company

Inventors

• Edmond Kazem V
• Perkins David L
• Mendez Daniella

Classifications

• G01N33/2823 Primary

  Raw oil, drilling fluid or polyphasic mixtures · CPC title

• G01N21/84

  Systems specially adapted for particular applications · CPC title

• G01N2021/6421

  Measuring at two or more wavelengths · CPC title

• G01N2021/6419

  Excitation at two or more wavelengths · CPC title

• G01N21/6456

  Spatial resolved fluorescence measurements; Imaging · CPC title