# US 11,111,445 B2 · Separation system for high pressure processing system

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- Number: US 11,111,445 B2
- Document ID: US11111445B2
- Status: Granted
- Kind: B2
- Application number: 16/499,010
- Filed: 2018-03-22
- Published: 2020-02-20
- Granted: 2021-09-07
- Earliest claimed: 2017-03-30
- Assignees: Steeper Energy Aps
- Applicants: Steeper Energy Aps
- Inventors: Steen Brummerstedt Iversen; Claus Uhrenholt Jensen; Göran Olofsson; Julie Katerine Rodriguez Guerrero; Andrew Ironside; Sergios Karatzos; Ling Li
- Web page: https://patentgrep.com/patent/US11111445B2

## CPC

- C10G 1/083: {in the presence of a solvent}
- C10G 31/06: by heating, cooling, or pressure treatment
- C10G 1/00: Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal (mechanical winning of oil from oil-shales, oil-sand, or the like B03B)
- C10G 17/02: with acids or acid-containing liquids, e.g. acid sludge
- C10G 31/08: by treating with water
- C10G 33/00: Dewatering or demulsification of hydrocarbon oils (by distillation C10G7/04)
- C10G 53/10: including at least one acid-treatment step
- C10G 67/14: including at least two different refining steps in the absence of hydrogen
- C10G 2300/1014: of vegetal origin
- C10G 2300/302: Viscosity
- C10G 2300/308: Gravity, density, e.g. API
- Y02P 30/20: using bio-feedstock
- 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
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

The invention relates to a method of separating and purifying products from a high pressure processing system adapted for processing a feed stream comprising carbonaceous material at a pressure of at least 150 bar and a temperature of at least 300° C., where the converted feed stream (product mixture) is cooled to a temperature in the range 50 to 250° C., and depressurized to a pressure in the range 1 to 150 bar, the method comprising separating the depressurized product mixture in gas phase, an oil phase (liquid hydrocarbon), and a water phase comprising water soluble organics, dissolved salts and optionally suspended particles in a first phase separator and purifying the oil phase from the first phase separator by mixing it with one or more washing agents, at least one of which comprises water, and separating the oil phase from the one or more washing agents in a further separation step.

## Claims

### Claim 1

Method of separating and purifying products from a high pressure processing system adapted for processing a feed stream comprising carbonaceous material at a pressure of at least 150 bar and a temperature of at least 300° C., where converted feed stream is cooled to a temperature in the range 50 to 250° C., and depressurized to a pressure in the range 1 to 150 bar, the method comprising:
separating the depressurized, converted feed stream into a gas phase, an oil phase, and a water phase comprising water soluble organics, dissolved salts and optionally suspended particles in a first phase separator; and
purifying the oil phase from the first phase separator by mixing it with one or more washing agents, and separating the oil phase from the one or more washing agents in at least one further separation step,
wherein gas is separated from the converted feed stream in a flash separator prior to entering the first phase separator, and the pressure of the flash separator is in the range 1 to 150 bar, and
wherein an acidifying agent is added to at least one of the one or more washing agents comprising water, and the acidifying agent comprises CO2 containing process gas.

### Claim 2 (depends on 1)

Method of separating and purifying products from a high pressure processing system according to claim 1, where the converted feed stream is depressurized to a pressure in the range 10 to 150 bar prior to the first phase separator.

### Claim 3 (depends on 1)

Method according to claim 1, where the at least one further separation step comprises the use of one or more phase separators, and where in each of such phase separation steps the oil phase is separated from at least one washing agent added to the oil phase prior to entering the additional phase separation step.

### Claim 4 (depends on 3)

Method according to claim 3, where the weight ratio to oil of said one or more washing agents, which are added to the oil phase prior to entering each of the at least one further separation steps, is in the range 0.01 to 2.0.

### Claim 5 (depends on 3)

Method according to claim 3, where the operating pressure of the one or more separators in the at least one further separation step is in the range 1 to 74 bar.

### Claim 6 (depends on 3)

Method according to claim 3, where the temperature in the first separator and/or in each of the separators in the at least one further separation step is/are in the range 120 to 200° C.

### Claim 7 (depends on 3)

Method according to claim 3, where the residence time in the first separator and/or in each of the separators in the at least one further separation step is/are in the range 0.1 to 30 minutes.

### Claim 8 (depends on 3)

Method according to claim 3, where the oil obtained from the at least one further separation step is flashed thereby producing a gas stream comprising low boiling hydrocarbons and water and an oil stream.

### Claim 9 (depends on 8)

Method according to claim 8, where the temperature of the flash of the oil obtained from the at least one further separation step is in the range 80 to 150° C.

### Claim 10 (depends on 8)

Method according to claim 8, where the gas stream from said flash of the oil obtained from the at least one further separation step is condensed and further separated into a light hydrocarbon liquid phase, a gas phase and a water phase.

### Claim 11 (depends on 10)

Method according to claim 10, where the separated light hydrocarbon phase is at least partly recycled and mixed with the oil phase from the first separator prior to entering the one or more separators in the at least one further separation step.

### Claim 12 (depends on 10)

Method according to claim 10, where the separated light hydrocarbon phase is at least partly mixed with the separated oil phase resulting from the flash of the oil obtained from the at least one further separation step.

### Claim 13 (depends on 3)

Method according to claim 3, where the liquid phase comprising washing agent(s) withdrawn from the one or more phase separators in the at least one further separation step is at least partly recycled and mixed with the oil phase from the previous separator prior to entering the subsequent separator in the further separation step.

### Claim 14 (depends on 1)

Method according to claim 1, where the amount of acidifying agent(-s) is selected so that the pH of the separated washing water from each of the at least one further separation step is in the range from about 2.0 to about 7.0.

### Claim 15 (depends on 1)

Method according claim 1, where the pressure of the flash separator is in the range 10 to 150 bar.

### Claim 16 (depends on 1)

Method according to claim 1, where dynamic viscosity of the oil phase during said separation and purification is in the range 0.1 to 30 cP.

### Claim 17 (depends on 1)

Method according to claim 1, where the one or more washing agents comprises or further comprises a viscosity and/or density reducing agent having a boiling point of less than 160° C.

### Claim 18 (depends on 17)

Method according to claim 17, where the viscosity and/or density reducing agent comprises:
one or more ketones, and/or acetone, and/or propanones; and
2-heptanone, and/or buthanones, and/or pentanones, and/or pentenones, and/or cyclopentanonees, and/or hexanones, and/or cyclohexanones, and/or heptanones, and/or one or more alcohols, and/or one or more aromatic compounds, and/or one or more alkanes.

### Claim 19 (depends on 17)

Method according to claim 17, where the viscosity and/or density reducing agent(-s) comprises one or more ketones in a concentration in the range 30-60% by weight, and one or more alcohols in a concentration in the range 5-30% by weight, and one or more aromatics in a concentration in the range 10 to 40% by weight, and one or more alkanes in the concentration in the range 10 to 30% by weight.

### Claim 20 (depends on 17)

Method according to claim 17, where the viscosity and/or density reducing agent comprises a low boiling point fraction of the oil from the converted feed mixture comprising carbonaceous material.

### Claim 21 (depends on 17)

Method according to claim 17, where the weight ratio of the viscosity reducing and/or density agent added to the amount of oil is in the range 0.01 to 2.

### Claim 22 (depends on 1)

Method according to claim 1, where the operating pressure of the first separator is in the range 1 to 74 bar.

### Claim 23 (depends on 1)

Method according to claim 1, where part of the oil phase is withdrawn after the first separator and recycled to prepare the feed stream to be processed by the high pressure processing system.

### Claim 24 (depends on 1)

Method according to claim 1, where the one or more washing agents comprises an emulsion breaker.

### Claim 25 (depends on 24)

Method according to claim 24, where said emulsion breaker comprises one or more solvents selected from the group of water, xylenes, ethanol, methanol, propanol, buthanol, toluene, phenol-formaldehyde resin, heavy and light aromatic naphtha, ethylbenzene, 1,2,4 trimethylbenzene, 1,3,5 trimethylbenzene, 1,2,3 trimethylbenzene, glutaraldehyde, 2-butanone, ethyl acetate, 1-propyl acetate, polymers of ethylene oxide, pentylamine, and butyl acrylate.

### Claim 26 (depends on 24)

Method according to claim 24, where the emulsion breaker comprises three or more solvents.

### Claim 27 (depends on 24)

Method according to claim 24, where the concentration of the emulsion breaker is in the range of 100 to 20000 ppm by weight.

### Claim 28 (depends on 24)

Method according to claim 24, where at least a majority of the emulsion breaker remains in the oil phase after separation of the oil from the one or more washing agents.

### Claim 29 (depends on 1)

Method according to claim 1, where the oil from the separation or at least a fraction thereof is further subjected to an upgrading process, where it is pressurized to a pressure in the range from about 20 bar to about 200 bar; and subsequently mixed with hydrogen and heated to a temperature in the range 250 to 400° C. in one or more steps, and contacted with one or more hydro-treating and/or hydro-processing and/or hydrocracking catalysts in one or more reaction zones, and optionally separated into different boiling point fractions.

### Claim 30 (depends on 29)

Method according to claim 29, where the oil is further subjected to an ion exchange step prior to said upgrading process.

### Claim 31 (depends on 30)

Method according to claim 30, where the ion exchange step uses one or more cation resins.