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EP0066477A2 Expired / Lapsed EP ⏱️ 0.0 years remaining

Process for producing a mesophase pitch and a carbon fiber by high pressure treatment of a precursor material

Assignee: Union Carbide Chemicals and Plastics Technology LLC
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Filing: 1982-03-26
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Granted: —
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Expires: 2002-03-26
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Abstract

Abstract The invention deals with a process for producing a mesophase pitch and a carbon pitch by high-pressure treatment of a precursor material. …<??>The process includes the steps of heat treating a selected precursor material under high pressure, thereafter solvent extracting the treated precursor material to obtain mesophase pitch, spinning the mesophase pitch into at least one pitch fiber, and converting the pitch fiber into carbon fiber. …<??>This high-pressure treatment provides a better yield of mesophase pitch having a relatively narrow molecular weight distribution, useful in spinning operations for good quality carbon fibers.

Inventors

  • 👤 Irwin Charles Lewis
  • 👤 Arthur William Moore

Bibliographic Details

Application Number —
Jurisdiction EP
Data Source google_patents
Last Synchronized 2026-11-08 20:20
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; D01F9/12; D01F9/14; D01F9/32; D01F9/322; D01F9/145

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 212 words
A process for producing carbon fiber, characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least about 50; by weight which boils under about 300°C and at least 70% by weight which boils under about 360°C; subjecting the material to a thermal-pressure treatment as a batch treatment for a temperature from about 400°C to about 475°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to obtain a precursor pitch; solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 2
Dependent Claim 212 words
A process for producing carbon fiber, characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least about 50; by weight which boils under about 300°C and at least 70% by weight which boils under about 360°C; subjecting the material to a thermal-pressure treatment as a batch treatment for a temperature from about 400°C to about 475°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to obtain a precursor pitch; solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 3
Dependent Claim 208 words
A process for producing a carbon fiber, characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least 50% by weight which boils under about 300°C and at least about 70% by weight which boils under 360°C; subjecting the material to a continuous treatment for a temperature from about 420°C to about 550°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to produce a precursor pitch; solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least about 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 4
Dependent Claim 208 words
A process for producing a carbon fiber, characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least 50% by weight which boils under about 300°C and at least about 70% by weight which boils under 360°C; subjecting the material to a continuous treatment for a temperature from about 420°C to about 550°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to produce a precursor pitch; solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least about 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 5
Dependent Claim 195 words
Process for producing a mesophase pitch characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least about 50% by weight which boils under about 300°C and at least 70% by weight which boils under about 360°C; subjecting the material to a thermal-pressure treatment as a batch treatment for a temperature from about 400°C to about 475°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to obtain a precursor pitch; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75 % of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least 70% by weight mesophase.
Claim 6
Dependent Claim 195 words
Process for producing a mesophase pitch characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least about 50% by weight which boils under about 300°C and at least 70% by weight which boils under about 360°C; subjecting the material to a thermal-pressure treatment as a batch treatment for a temperature from about 400°C to about 475°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to obtain a precursor pitch; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75 % of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least 70% by weight mesophase.
Claim 7
Dependent Claim 190 words
A process for producing a mesophase pitch, characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least 50% by weight which boils under about 300°C and at least about 70% by weight which boils under 360°C;- subjecting the material to a continuous treatment for a temperature-from about 420°C to about 550°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to produce a precursor pitch; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75 % of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15X of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least about 70% by weight mesophase.
Claim 8
Dependent Claim 190 words
A process for producing a mesophase pitch, characterized in that it comprises the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, aromatic hydrocarbons, and coal tar distillates having at least 50% by weight which boils under about 300°C and at least about 70% by weight which boils under 360°C;- subjecting the material to a continuous treatment for a temperature-from about 420°C to about 550°C and for a gauge pressure from about 1.38 MPa to about 10.35 MPa to produce a precursor pitch; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75 % of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15X of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least about 70% by weight mesophase.
Claim 9
Dependent Claim 27 words
The process according to any one of claims 1 or 3, wherein the soaking volume factor for the thermal-pressure treatment is from about 0.4 to about 8.6.
Claim 10
Dependent Claim 34 words
The process of claim 5, wherein the thermal-pressure treatment is continued until the Conradson carbon content of the precursor pitch is from about 20% to about 65% and is preferably at least about 30%.
Claim 11
Dependent Claim 26 words
The process of claim 6, wherein the thermal-pressure treatment is carried out with the material being agitated, preferably the agitation being in the form of stirring.
Claim 12
Dependent Claim 32 words
The process according to the claims 1 and 6 taken in combination, characterized in that it further comprises filtering the precursor pitch prior to the solvent extracting step to remove infusible solids.
Claim 13
Dependent Claim 29 words
The process of claim 6, further comprising distilling the precursor pitch to raise its softening point to a predetermined temperature, preferably the said temperature being at least about 120°C.
Claim 14
Dependent Claim 27 words
The process according to any one of claims 2 or 4, wherein the soaking volume factor for the continuous treatment is from about 0.4 to about 2.6.
Claim 15
Dependent Claim 35 words
The process of claim 10, wherein the continuous treatment is carried out until the Conradson carbon content of the precursor pitch is from about 5% to about 65% and is preferably at least about 10%.
Claim 16
Dependent Claim 20 words
The process of claim 11, further comprising distilling the precursor pitch to raise its softening point to a predetermined temperature.
Claim 17
Dependent Claim 33 words
The process according to any one of claims 9 or 12, wherein the distilling step is carried out to raise the Conradson carbon content of the precursor pitch to at least about 40%.

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