# US 4,391,699 A · Coal liquefaction process

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- Number: US 4,391,699 A
- Document ID: US4391699A
- Status: Granted
- Kind: A
- Application number: 06/345,281
- Filed: 1982-02-03
- Granted: 1983-07-05
- Earliest claimed: 1976-12-27
- Assignees: Chevron Research Company
- Inventors: Joel W. Rosenthal
- Web page: https://patentgrep.com/patent/US4391699A

## CPC

- C10G 47/00: Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions (C10G15/00 takes precedence; destructive hydrogenation of non-melting solid carbonaceous or similar materials C10G1/06)
- C10G 1/002: {in combination with oil conversion- or refining processes}
- C10G: CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION (cracking to hydrogen or synthesis gas C01B; cracking or pyrolysis of hydrocarbon gases to individual hydrocarbons or mixtures thereof of definite or specified constitution C07C; cracking to cokes C10B); RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES

## Abstract

Disclosed is a two-stage process for the production of liquid hydrocarbons from coal. More particularly, disclosed is a two-stage coal liquefaction process wherein subdivided coal is substantially dissolved in a solvent in a first non-catalytic dissolving stage at the temperature in the range 750.degree. to 900.degree. F. In a second stage, the mixture of solvent, dissolved coal and insoluble solids is contacted with a hydrocracking catalyst at a critical temperature below 800.degree. F. The normally liquid portion of the hydrocracker effluent product has a surprisingly low sulfur content of less than 0.1 weight percent, a low nitrogen content of less than 0.5 weight percent, and a high API gravity of at least -3.

## Claims

### Claim 1

A process for liquefying coal comprising:
(a) mixing subdivided coal with a solvent to form a coal-solvent slurry;
(b) heating said slurry in a dissolving zone to a temperature in the range of 750.degree.-900.degree. F. at a pressure above 500 psig in the presence of added hydrogen to form a first effluent comprising normally liquid components, non-distillable oil components, and undissolved solids;
(c) passing at least a portion of said first effluent into a reaction zone, said portion comprising non-distillable oil components, and contacting said portion with hydrogen in the presence of an externally provided hydrogenation catalyst under hydrogenation conditions, including a temperature below 800.degree. F. and lower than the temperature in said dissolving zone;
(d) withdrawing a second effluent from said reaction zone, said second effluent comprising normally liquid components and non-distillable oil components; and
(e) recycling at least a portion of said second effluent to step (a), said recycle portion comprising both normally liquid components and non-distillable oil components.

### Claim 2 (depends on 1)

The process according to claim 1 wherein substantially all of said normally liquid components and said non-distillable oil components from said dissolving zone are passed into said reaction zone.

### Claim 3 (depends on 1)

The process according to claim 1 wherein said portion of said first effluent comprises a full boiling range portion of said normally liquid components and said non-distillable oil components.

### Claim 4 (depends on 3)

The process according to claim 3 wherein substantially all of said non-distillable oil components from said dissolving zone are passed into said reaction zone.

### Claim 5 (depends on 1, 2, 3)

The process according to claim 1, 2, 3, or 4 wherein said coal-solvent slurry is heated in said dissolving zone in the absence of an externally supplied catalyst or contact particles.

### Claim 6 (depends on 1, 2, 3)

The process according to claim 1, 2, 3, or 4 wherein said step (c) comprises passing said portion of said first effluent mixture upwardly through a fixed bed comprising said hydrogenation catalyt.

### Claim 7 (depends on 1, 2, 3)

The process according to claim 1, 2, 3, or 4 wherein said hydrogenation catalyst comprises one or more elements selected from Group VIB and Group VIII on a refractory oxide support comprising material selected from the group consisting of alumina, silica-alumina, silica-magnesia, silica-zirconia, alumina-boria, silica-titania, silica-zirconia-titania, and acid-treated clays.

### Claim 8 (depends on 7)

The process according to claim 7 wherein said support is alumina.

### Claim 9 (depends on 1, 2, 3)

The process according to claim 1, 2, 3, or 4 wherein the temperature in said reaction zone is at least 100.degree. F. lower than the temperature in said dissolving zone.

### Claim 10 (depends on 1, 2, 3, 4)

The process according to claim 1, 2, 3 or 4 wherein the temperature in said reaction zone is at least 150.degree. F. lower than the temperature in said dissolving zone.

### Claim 11 (depends on 1, 2, 3)

The process according to claim 1, 2, 3, or 4 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 650.degree.-750.degree. F. and a pressure within the range of 1000 to 3000 psig.

### Claim 12 (depends on 5)

The process according to claim 5 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 650.degree.-750.degree. F. and a pressure within the range of 1000 to 3000 psig.

### Claim 13 (depends on 1, 2, 3)

The process according to claim 1, 2, 3, or 4 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 650.degree.-750.degree. F. and a pressure within the range of 1500 to 2500 psig.

### Claim 14 (depends on 5)

The process according to claim 5 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 650.degree.-750.degree. F. and a pressure within the range of 1500 to 2500 psig.

### Claim 15 (depends on 10)

The process according to claim 10 wherein said support is alumina.

### Claim 16

A process for liquefying coal comprising:
(a) mixing subdivided coal with a solvent to form a coal-solvent slurry, and solvent comprising non-distillable oil components;
(b) heating said slurry in a dissolving zone to a temperature in the range of 750.degree.-900.degree. F. at a pressure above 500 psig in the presence of added hydrogen to form a first effluent comprising normally liquid components, non-distillable oil components, and undissolved solids;
(c) passing at least a portion of said first effluent into a reaction zone, said portion comprising normally liquid components and non-distillable oil components, and contacting said portion with hydrogen in the presence of an externally provided hydrogenation catalyst under hydrogenation conditions, including a temperature below 800.degree. F. and lower than the temperature in said dissolving zone; and
(d) withdrawing a second effluent from said reaction zone, said second effluent containing normally liquid components and non-distillable oil components.

### Claim 17 (depends on 16)

The process according to claim 16 wherein substantially all of said normally liquid components and said non-distillable oil components from said dissolving zone are passed to said reaction zone.

### Claim 18 (depends on 16)

The process according to claim 16 wherein said portion of said first effluent comprises normally liquid components and is passed from said dissolving zone to said reaction zone without fractionation of normally liquid components in said first effluent.

### Claim 19 (depends on 16)

The process according to claim 16 wherein substantially all of said non-distillable oil components from said dissolving zone are passed to said reaction zone.

### Claim 20 (depends on 16, 17, 18, 19)

The process according to claim 16, 17, 18 or 19 wherein said coal-solvent slurry is heated in said dissolving zone in the absence of any externally supplied catalyst or contact particles.

### Claim 21 (depends on 16, 17, 18, 19)

The process according to claim 16, 17, 18 or 19 wherein said step (c) comprises passing said portion of said first effluent mixture upwardly through a fixed bed comprising said hydrogenation catalyst.

### Claim 22 (depends on 16, 17, 18)

The process according to claim 16, 17, 18, or 19 wherein said hydrogenation catalyst comprises one or more elements selected from Group VIB and Group VIII on a refractory oxide support comprising material selected from the group consisting of alumina, silica-alumina, silica-magnesia, silica-zirconia, alumina-boria, silica-titania, silica-zirconia-titania, and acid-treated clays.

### Claim 23 (depends on 16, 17, 18)

The process according to claim 16, 17, 18, or 19 wherein the temperature in said reaction zone is at least 100.degree. F. lower than the temperature in said dissolving zone.

### Claim 24 (depends on 16, 17, 18)

The process according to claim 16, 17, 18, or 19 wherein the temperature in said reaction zone is at least 150.degree. F. lower than the temperature in said dissolving zone.

### Claim 25 (depends on 16, 17, 18)

The process according to claim 16, 17, 18, or 19 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 750.degree.-850.degree. F. and a pressure within the range of 1000 to 3000 psig.

### Claim 26 (depends on 20)

The process according to claim 20 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 750.degree.-850.degree. F. and a pressure within the range of 1000 to 3000 psig.

### Claim 27 (depends on 16, 17, 18)

The process according to claim 16, 17, 18, or 19 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 750.degree.-850.degree. F. and a pressure within the range of 1500 to 2500 psig.

### Claim 28 (depends on 20)

The process according to claim 20 wherein said hydrogenation conditions in said reaction zone include a temperature within the range of 750.degree.-850.degree. F. and a pressure within the range of 1500 to 2500 psig.
