# US 10,871,323 B2 · Method of liquefying a CO2 contaminated hydrocarbon-containing gas stream

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- Number: US 10,871,323 B2
- Document ID: US10871323B2
- Status: Granted
- Kind: B2
- Application number: 15/779,634
- Filed: 2016-12-01
- Published: 2018-12-06
- Granted: 2020-12-22
- Earliest claimed: 2015-12-03
- Assignees: Shell Oil Company
- Applicants: Shell Oil Company
- Inventors: Thijs Groenendijk; Raimo Edwin Gregor Poorte; Nirupa Raghavan; Michiel Gijsbert Van Aken
- Web page: https://patentgrep.com/patent/US10871323B2

## CPC

- F25J 3/067: {separation of carbon dioxide (production of carbon dioxide in general C01B32/00)}
- F25J 1/0022: {Hydrocarbons, e.g. natural gas}
- F25J 1/0035: {by gas expansion with extraction of work}
- F25J 1/0037: {of a return stream}
- F25J 1/004: {by flash gas recovery (F25J1/0267 takes precedence)}
- F25J 1/0202: {in a quasi-closed internal refrigeration loop (F25J1/0208, F25J1/0219, F25J1/0224 take precedence)}
- F25J 1/0209: {as at least a three level refrigeration cascade}
- F25J 1/021: {using a deep flash recycle loop}
- F25J 3/061: {Natural gas or substitute natural gas}
- F25J 3/0635: {separation of CnHm with 1 carbon atom or more}
- F25J 2205/10: using combined expansion and separation, e.g. in a vortex tube, "Ranque tube" or a "cyclonic fluid separator", i.e. combination of an isentropic nozzle and a cyclonic separator; Centrifugal separation
- F25J 2205/20: using solidification of components
- F25J 2205/30: using a washing, e.g. "scrubbing" or bubble column for purification purposes
- F25J 2205/90: Mixing of components
- F25J 2210/04: Mixing or blending of fluids with the feed stream
- F25J 2215/04: Recovery of liquid products
- F25J 2220/66: Separating acid gases, e.g. CO2, SO2, H2S or RSH
- F25J 2220/82: Separating low boiling, i.e. more volatile components, e.g. He, H2, CO, Air gases, CH4
- F25J 2230/30: Compression of the feed stream
- F25J 2230/60: the fluid being hydrocarbons or a mixture of hydrocarbons
- F25J 2235/60: the fluid being (a mixture of) hydrocarbons
- F25J 2235/80: the fluid being carbon dioxide
- F25J 2240/02: Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
- F25J 2245/02: Recycle of a stream in general, e.g. a by-pass stream
- F25J 2245/90: the recycled stream being boil-off gas from storage
- F25J 2270/04: Internal refrigeration with work-producing gas expansion loop
- F25J 2270/88: Quasi-closed internal refrigeration or heat pump cycle, if not otherwise provided
- Y02C 20/40: of CO2
- F25J: LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS {OR LIQUEFIED GASEOUS} MIXTURES BY PRESSURE AND COLD TREATMENT {OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE (cryogenic pumps F04B37/08; gas storage vessels, gas holders F17; filing vessels with, or discharging from vessels, compressed, liquefied or solidified gases F17C; refrigeration machines, plants, or systems F25B)}
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]

## Abstract

The present invention provides a method of liquefying a contaminated hydrocarbon-containing gas stream: (a) providing a CO2 contaminated hydrocarbon-containing gas stream (20); (b) cooling the contaminated hydrocarbon-containing gas stream to obtain a partially liquefied stream (70); (c) separating the partially liquefied stream obtaining a liquid stream (90); (d) cooling the liquid stream (90) in a direct contact heat exchanger (200) obtaining a multiphase stream (201) containing at least a liquid phase and a solid CO2 phase; (e) separating the multiphase stream in a solid-liquid separator (202) obtaining a CO2 depleted liquid stream (141); (f) passing the CO2 depleted liquid stream (141) to a further cooling, pressure reduction and separation stage to generate a further CO2 enriched slurry stream (206); (g) passing at least part of the further CO2 enriched slurry stream (206) to the direct contact heat exchanger (200) to provide cooling duty to and mix with the liquid stream (90).

## Claims

### Claim 1

A method of liquefying a contaminated hydrocarbon-containing gas stream, the method comprising at least the steps of:
(a) providing a contaminated hydrocarbon-containing gas stream having a contaminant being carbon dioxide (CO2);
(b) cooling the contaminated hydrocarbon-containing gas stream to produce a partially liquefied stream;
(c) separating the partially liquefied stream in a separator thereby producing a gaseous stream and a liquid stream;
(d) cooling the liquid stream produced in step (c) by passing the liquid stream to a direct contact heat exchanger thereby producing a multiphase stream, the multiphase stream containing at least a liquid phase and a solid phase, the solid phase containing CO2 particles;
(e) separating the multiphase stream in a solid-liquid separator thereby producing a CO2 depleted liquid stream and a first CO2 enriched slurry stream;
(f) passing the CO2 depleted liquid stream to a cooling, pressure reduction, and separation stage, the cooling, pressure reduction and separation stage generating a gaseous stream, a purified liquid stream, and a second CO2 enriched slurry stream;
(g) passing at least part of the second CO2 enriched slurry stream to the direct contact heat exchanger to provide cooling duty to and mix with the liquid stream produced in step (c).

### Claim 2 (depends on 1)

The method according to claim 1, wherein the solid phase of the multiphase stream produced in step (d) contains CO2 particles with an average diameter greater than 50 micron.

### Claim 3 (depends on 1)

The method according to claim 1, wherein molecules forming the liquid stream produced in step (c) and molecules forming the at least part of the second CO2 enriched slurry stream produced in step (f) in the direct contact heat exchanger have residence times greater than 10 seconds.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the passing the liquid stream produced in step (c) to the direct contact heat exchanger comprises passing the liquid stream over a pressure reduction device.

### Claim 5 (depends on 1)

The method according to claim 1, wherein a pressure and a temperature in the direct contact heat exchanger are selected so that a vapor phase, a liquid phase and a solid phase are present simultaneously.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the solid-liquid separator of step (e) comprises one or more cyclone separators, one or more filters, or one or more gravity based settling vessels.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the passing the CO2 depleted liquid stream to the cooling, pressure reduction, and separation stage of step (f) comprises:
(f1) passing the CO2 depleted liquid stream over a pressure reduction device and into a separator,
and wherein the generating of step (f) comprises:
(f2) producing the gaseous stream as a top stream from the separator and producing a different multiphase stream as a bottom stream from the separator, the different multiphase stream containing at least a liquid phase and a solid phase, the solid phase containing CO2 particles,
(f3) separating the different multiphase stream in a different solid-liquid separator thereby producing the purified liquid stream and the second CO2 enriched slurry stream.

### Claim 8 (depends on 7)

The method according to claim 7, wherein the pressure reduction device is a Joule Thomson valve.

### Claim 9 (depends on 1)

The method according to claim 1 further comprising:
(h) passing the purified liquid stream to an end flash stage producing an end flash gas stream and a liquid natural gas stream.

### Claim 10 (depends on 9)

The method according to claim 9, wherein a portion of the liquid natural gas stream is fed back to the cooling, pressure reduction and separation stage of step (f) to provide cooling duty to the CO2 depleted liquid stream.

### Claim 11 (depends on 10)

The method according to claim 10, wherein the portion of the liquid natural gas stream is mixed with the different multiphase stream produced in step (f2) upstream of the different solid-liquid separator of step (f3).

### Claim 12 (depends on 11)

The method according to claim 11, wherein mixing of the portion of the liquid natural gas stream and the different multiphase stream is done in a different direct contact heat exchanger.

### Claim 13 (depends on 1)

The method according to claim 1, wherein the cooling of step (b) comprises:
(b1) cooling the contaminated hydrocarbon-containing gas stream in a first heat exchanger thereby producing a cooled contaminated hydrocarbon-containing stream,
(b2) cooling the cooled contaminated hydrocarbon-containing stream in an expander thereby producing the partially liquefied stream.

### Claim 14 (depends on 1)

The method according to claim 1, wherein the solid phase of the multiphase stream produced in step (d) contains CO2 particles with an average diameter greater than 100 micron.

### Claim 15 (depends on 1)

The method according to claim 1, wherein the solid phase of the multiphase stream produced in step (d) contains CO2 particles with an average diameter greater than 350 micron.

### Claim 16

A system for liquefying a contaminated hydrocarbon-containing gas stream, the system comprising:
(a) a feed conduit arranged to provide a contaminated hydrocarbon-containing gas stream-having a contaminant being carbon dioxide (CO2);
(b) a cooling stage arranged to receive the contaminated hydrocarbon-containing gas stream and discharge a partially liquefied stream;
(c) a separator arranged to receive the partially liquefied stream and to discharge a gaseous stream and a liquid stream;
(d) a direct contact heat exchanger arranged to receive and cool the liquid stream produced in step (c) to produce a multiphase stream, the multiphase stream containing at least a liquid phase and a solid phase, the solid phase containing CO2 particles;
(e) a solid-liquid separator arranged to receive the multiphase stream and discharge a CO2 depleted liquid stream and a CO2 enriched slurry stream;
(f) a cooling, pressure reduction and separation stage arranged to receive the CO2 depleted liquid stream and generate a gaseous stream, a purified liquid stream and a second CO2 enriched slurry stream;
(g) a recycle conduit which is arranged to pass at least part of the second CO2 enriched slurry stream comprising solid CO2 particles to the direct contact heat exchanger to provide cooling duty to and mix with the liquid stream produced by the separator.