Search

JP-7857419-B2 - Pitch composition and method relating to the pitch composition

JP7857419B2JP 7857419 B2JP7857419 B2JP 7857419B2JP-7857419-B2

Inventors

  • パーキンス，デイビッド エル
  • スミス，スチュアート イー
  • パテル，ネビル
  • チェイス，クラレンス イー
  • アフェウォルキ，モバエ

Assignees

  • エクソンモービル テクノロジー アンド エンジニアリング カンパニー

Dates

Publication Date
20260512
Application Date
20230323
Priority Date
20220328

Claims (20)

  1. A composition comprising a pitch composition having both an A-factor in the range of approximately 0.4 to approximately 0.8 and an aromaticity in the range of approximately 0.3 to approximately 0.7.
  2. The composition according to claim 1, wherein the A-factor is in the range of about 0.6 to about 0.8, and the aromaticity is in the range of about 0.3 to about 0.6.
  3. The composition according to claim 1 or 2, further comprising a softening point in the range of approximately 90°C to approximately 150°C and less than approximately 20% by volume of mesophase.
  4. The composition according to claim 1, wherein the A-factor is in the range of about 0.4 to about 0.6, and the aromaticity is in the range of about 0.5 to about 0.7 .
  5. The composition according to any one of claims 1, 2, or 4, further comprising a softening point in the range of approximately 250°C to approximately 350°C and more than approximately 30% by volume of mesophase.
  6. The composition according to any one of claims 1, 2, or 4, further comprising a softening point in the range of approximately 150°C to approximately 350°C and more than approximately 50% by volume of mesophase.
  7. The composition according to claim 1, wherein the pitch composition comprises a blend of pitches including at least a first pitch composition and a second pitch composition.
  8. At least the first pitch composition and the second pitch composition are thermally decomposed. Here, the thermal decomposition of the first pitch composition and the second pitch composition is carried out separately. The first pitch composition is a composition derived from the first pitch feed, The aforementioned second pitch composition is a composition derived from the second pitch feed, Obtain a first infrared spectrum of at least a first pitch composition, and select at least one first infrared parameter based on (1) the first infrared spectrum and a calibration curve or (2) the first infrared spectrum and chemometric modeling. A method comprising: obtaining a second infrared spectrum of at least a second pitch composition; selecting at least one second infrared parameter based on (1) the second infrared spectrum and a calibration curve or (2) the second infrared spectrum and chemometric modeling, wherein the selected first and second infrared parameters are at least one or both of an A-factor in the range of about 0.4 to about 0.8 and/or aromaticity in the range of about 0.3 to about 1.3; and blending the first and second pitch compositions in a ratio that achieves the selected first and second infrared parameters, thereby forming a blended pitch composition.
  9. The method according to claim 8, wherein the selected first and second infrared parameters further include a softening point in the range of about 90°C to about 150°C and less than about 20% by volume of mesophase.
  10. The method according to claim 8, wherein the selected first and second infrared parameters further include a softening point in the range of about 250°C to about 350°C and a mesophase exceeding about 30% by volume.
  11. The method according to claim 8, wherein the selected first and second infrared parameters further include a softening point in the range of about 150°C to about 350°C and a mesophase exceeding about 50% by volume.
  12. The method according to any one of claims 8 to 11, further comprising using blended pitch to spin or manufacture one or both carbon fibers and/or carbon fiber composite materials.
  13. The method according to any one of claims 8 to 11, further comprising using blended pitch to produce one or more of mesocarbon microbeads, graphite, and/or needle coke.
  14. Before thermal decomposition, Obtain a first initial infrared spectrum of a first pitch feeder, and select at least one first initial infrared parameter based on (1) the first initial infrared spectrum and a calibration curve, or (2) the first initial infrared spectrum and chemometric modeling. The method according to claim 8, further comprising: obtaining a second initial infrared spectrum of a second pitch feeder; (1) selecting at least one second initial infrared parameter based on the second initial infrared spectrum and a calibration curve, or (2) the second initial infrared spectrum and chemometric modeling, wherein the selected first and second initial infrared parameters are either or both of the initial A-factor and/or initial aromaticity, except in the range of about 0.4 to about 0.8 and/or the range of about 0.3 to about 1.3.
  15. The method according to claim 14, further comprising the thermal decomposition of contacting the first and second pitch feeds with a reactive gas at a temperature in the range of about 200°C to about 600°C and a pressure exceeding 0.3 psi, thereby producing a first pitch spill containing the first pitch composition and a second pitch spill containing the second pitch composition.
  16. After pyrolysis, The method further includes separating a first pitch composition from a first pitch spill and separating a second pitch composition from a second pitch spill. The method according to claim 15, wherein the separation is selected from distillation separation, deasphalt separation, membrane separation, or any combination thereof.
  17. The method according to claim 15 or 16, wherein the reactive gas is selected from the group consisting of hydrogen, air, oxygen, ozone, hydrogen peroxide, carbon monoxide, carbon dioxide, formic acid, nitrogen dioxide, and any combination thereof.
  18. To extrude a pitch composition to produce green carbon fibers, and then to stabilize the extruded pitch composition. Here, stabilization includes obtaining an infrared spectrum of the extruded pitch composition and selecting at least one infrared parameter based on (1) a first infrared spectrum and a calibration curve, or (2) a first infrared spectrum and chemometric modeling. Here, at least one infrared parameter is at least the A-factor and aromaticity, and when the A-factor is in the range of about 0.4 to about 0.8 and/or aromaticity is in the range of about 0.3 to about 1.3, A method that includes stopping stabilization.
  19. The method according to claim 18, wherein a pitch composition is extruded through a spinneret, and the method further comprises spooling the extruded pitch composition before stabilization, wherein the stabilization is performed using a reactive gas.
  20. The method according to claim 18, wherein the extrusion comprises blowing a pitch composition through an extrusion die.

Description

This disclosure relates to pitch compositions, and more particularly to the properties of controlled pitch compositions and methods for their manufacture and use. Pitch is a carbon-containing raw material that can be classified as either isotropic pitch or mesophase pitch. Both isotropic and mesophase pitches can be complex mixtures of aromatic molecules, but while the aromatic molecules in isotropic pitch are randomly oriented, in mesophase pitch at least some of these aromatic molecules are ordered. Mesophase pitch may have a heterogeneous two-phase structure containing the ordered aromatic molecules (e.g., anisotropic regions) and isotropic regions. Generally, the formation of isotropic pitch precedes the formation of mesophase pitch. In this specification, unless otherwise specified, both types of pitch are collectively referred to as "pitch." Pitch can be produced from acid-catalyzed oligomerization of raw materials such as petroleum, coal tar, biomaster, or low molecular weight materials (e.g., naphthalene). Typical chemical components of pitch include, but are not limited to, alkanes, cycloalkanes, aromatics, hydroaromatics, phenols, alkenes, ketones, carboxylic acids, sulfur-containing compounds, oxygen-containing compounds, and nitrogen-containing compounds. These components vary depending on the starting materials and process conditions. Pitch is used in a wide range of product applications, including carbon fibers, binder pitch, and impregnation pitch. Major markets for pitch include, but are not limited to, high-performance and general-purpose carbon fibers, refractories, carbon/carbon composite materials, artificial graphite, graphite components, binders and impregnation pitch for electrodes, binders and impregnation pitch for anodes and cathodes in aluminum manufacturing, impregnation pitch for electric furnace electrodes in steelmaking, mesocarbon microbeads for anodes in lithium-ion batteries, carbon foam for thermal conductivity applications¹¹ ,¹³ and sound absorption applications, roofing products, lubricants, and consumer products (such as cosmetics). Given the chemical diversity of pitch, its properties depend on, but are not limited to, its raw materials, manufacturing (e.g., pyrolysis), and separation (e.g., distillation) conditions. Different pitch properties are specified for specific end-uses, each with its own defined range of acceptable specifications. These include, but are not limited to, the softening point, microcarbon residue (or residue, or remainder), mesophase percentage (%), and other applicable property ranges. However, currently, there is no way to predict or control these properties, and the typical method for obtaining pitch property specifications suitable for a particular end-use is simply trial and error and based on past experience, which is at least costly in terms of manufacturing time and raw materials (such as pitch material). Indeed, such a trial-and-error approach requires many experimental sets under multiple different conditions and product characteristics before the desired pitch properties are achieved. Significant research and development efforts have been expended to identify suitable supplies and processes for producing specific commercial pitches, such as ASHLAND A240, or suitable pitch blends, such as binder pitches, but this has proven impossible when the pitch raw materials are immutable. Furthermore, this trial-and-error approach does not consider the pitch composition and is only effective when the pitch composition is nearly constant. When a large market is desired for new pitch products such as carbon fiber composite materials for infrastructure applications, fluctuations in raw materials are unavoidable, and therefore the pitch composition fluctuates consistently, making the trial-and-error approach even more undesirable. Therefore, there is a strong need for methods to adjust the characteristics and enable the production of controlled pitch compositions with reproducible properties. In non-limiting embodiments of this disclosure, examples include compositions comprising a pitch composition having either or both an A-factor (or A-factor) in the range of about 0.4 to about 0.8 and/or an aromaticity (or aromaticity) in the range of about 0.3 to about 1.3. In a non-limiting aspect of this disclosure, a method is provided comprising thermally decomposing at least a first pitch composition and a second pitch composition, wherein the thermal decomposition of the first and second pitch compositions is carried out separately, the first pitch composition being a composition from a first pitch feed and the second pitch composition being a composition from a second pitch feed. A first infrared spectrum is obtained from at least the first pitch composition, and at least one first infrared parameter is selected based on (1) the first infrared spectrum and a calibration curve or (2) the first infrared spectrum and chemometric (or chemometric) modeling. A s