# US 11,898,101 B2 · Method and apparatus for continuous production of mesophase pitch

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- Number: US 11,898,101 B2
- Document ID: US11898101B2
- Status: Granted
- Kind: B2
- Application number: 17/300,591
- Filed: 2021-08-26
- Published: 2023-03-02
- Granted: 2024-02-13
- Earliest claimed: 2021-08-26
- Assignees: Koppers Delaware, Inc.
- Applicants: Koppers Delaware, Inc.
- Inventors: James T. Dietz
- Web page: https://patentgrep.com/patent/US11898101B2

## CPC

- C10C 3/02: by chemical means {reaction}
- B01J 4/008: {Feed or outlet control devices}
- B01J 19/0013: {Controlling the temperature of the process}
- B01J 19/006: {Baffles}
- B01J 19/18: Stationary reactors having moving elements inside (B01J19/08, B01J19/26 take precedence)
- B01J 19/1812: {Tubular reactors}
- B01J 19/1875: {internally, i.e. the mixture circulating inside the vessel such that the upwards stream is separated physically from the downwards stream(s)}
- C10C 3/002: {by thermal means}
- B01J 2219/00094: Jackets
- B01J 2219/00159: controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
- B01J 2219/00182: controlling the level of reactants in the reactor vessel
- B01J 2219/00189: controlling the stirring velocity
- B01J 2219/00763: Baffles
- B01J 2219/185: vertical
- C10C: WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID (compositions of bituminous materials C08L95/00; carbon filaments by decomposition of organic filaments D01F9/14)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

A process and apparatus for the continuous conversion of isotropic carbonaceous materials into anisotropic mesophase pitch is disclosed. The invention disclosed herein addresses the need for lower production costs compared with traditional batch mesophase conversion of isotropic pitch. A unique thermal processing and in-process separation of reacted mesophase from the continuous matrix of fresh or partially reacted isotropic pitch is provided. Potential uses are for further continuous processing into carbon fibers or carbon form densification.

## Claims

### Claim 1

An apparatus for continuous production of mesophase pitch comprising:
a generally cylindrical reactor vessel having an outer vessel wall, a top end and a bottom end, said vessel having an upper temperature zone and a lower temperature zone;
a reactor head mounted on said top end of said vessel;
a cylindrical tube baffle centered and mounted along a central axis of said vessel and spaced inwardly from said outer vessel wall forming (i) an inside space within said cylindrical tube baffle, (ii) an outside space between said cylindrical tube baffle and said outer vessel wall and (iii) a circulation path through said inside space and said outside space;
an inlet for feeding isotropic pitch into the upper temperature zone;
an agitator for circulating fluid along said circulation path in said vessel through said inside space and said outside space;
a mesophase separator located between said upper temperature zone and said lower temperature zone;
a first heating element for heating said upper temperature zone;
a second heating element for heating said lower temperature zone; and
an outlet for providing mesophase pitch for further processing.

### Claim 2 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said agitator is powered by a motor.

### Claim 3 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said agitator further comprises at least one axial flow impeller at an end of said inside space and at least one high-shear impeller within said inside space.

### Claim 4 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 further comprising at least one sparge ring to dispense an inert gas in a direction of fluid flow within said outside space.

### Claim 5 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said inlet further comprises a branch line to feed isotropic pitch to a second reactor vessel in parallel to said vessel.

### Claim 6 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said reactor head is flanged.

### Claim 7 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said bottom end of said outer vessel wall further comprises a conical bottom in which said lower temperature zone is located.

### Claim 8 (depends on 7)

An apparatus for continuous production of mesophase pitch according to claim 7 wherein said conical bottom is flanged.

### Claim 9 (depends on 8)

An apparatus for continuous production of mesophase pitch according to claim 8 wherein higher density mesophase material accumulates in said conical bottom of said vessel.

### Claim 10 (depends on 7)

An apparatus for continuous production of mesophase pitch according to claim 7 wherein said outlet is located in said conical bottom of said vessel.

### Claim 11 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said first and second heating elements are selected from the group consisting of radiant heaters, contact resistance heaters, induction heaters and molten salt or metal when an external jacket is employed.

### Claim 12 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said first heating element is configured to maintain said upper temperature zone at a temperature necessary to maintain reaction conditions.

### Claim 13 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said second heating element is configured to maintain said lower temperature zone at a temperature below that necessary to maintain reaction conditions but above that necessary to maintain mesophase pitch in a liquid state.

### Claim 14 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 further comprising one or more additional temperature zones to control reaction conditions more precisely.

### Claim 15 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 further comprising a transfer pump to extract mesophase pitch from said outlet.

### Claim 16 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein mesophase pitch exits said outlet by reactor operating pressure.

### Claim 17 (depends on 4)

An apparatus for continuous production of mesophase pitch according to claim 4 wherein at least one of said sparge ring and said agitator continuously circulates fluid including unreacted isotropic pitch from said lower temperature zone back to said upper temperature zone for further reaction.

### Claim 18 (depends on 1)

An apparatus for continuous production of mesophase pitch according to claim 1 wherein said inlet is located near said top end of said outer vessel wall.
