# US 10,441,898 B1 · Vertical integration of source water treatment

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- Number: US 10,441,898 B1
- Document ID: US10441898B1
- Status: Granted
- Kind: B1
- Application number: 15/731,637
- Filed: 2017-07-10
- Granted: 2019-10-15
- Earliest claimed: 2014-02-08
- Applicants: Mansour S. Bader
- Inventors: Mansour S. Bader
- Web page: https://patentgrep.com/patent/US10441898B1

## CPC

- B01D 17/047: {with separation aids}
- C02F 1/40: Devices for separating or removing fatty or oily substances or similar floating material (cleaning or keeping clear the surface of open water from oil or like materials E02B15/04; devices in sewers for separating liquid or solid substances from sewage E03F5/14, e.g. for use in drains leading to the sewer E03F5/16)
- B01D 3/065: {Multiple-effect flash distillation (more than two traps)}
- B01D 17/0205: {by gas bubbles or moving solids}
- B01D 19/0036: {Flash degasification (the other groups take precedence)}
- B01D 61/025: {Reverse osmosis; Hyperfiltration}
- B01D 61/027: {Nanofiltration}
- B01D 61/0271: {comprising multiple nanofiltration steps}
- B01D 61/029: {Multistep processes comprising different kinds of membrane processes selected from reverse osmosis, hyperfiltration or nanofiltration}
- B01D 61/04: Feed pretreatment
- B01D 61/58: Multistep processes
- B01D 69/02: characterised by their properties
- C02F 1/042: {Prevention of deposits}
- C02F 1/06: Flash evaporation
- C02F 1/44: by dialysis, osmosis or reverse osmosis {(general membrane separation processes B01D61/00, membrane modules B01D63/00, electrodialysis C02F1/4693, combination of membrane modules and bioreactors C02F3/1268)}
- C02F 1/5245: {using basic salts, e.g. of aluminium and iron}
- C02F 1/5272: {using specific organic precipitants}
- C02F 9/00: Multistage treatment of water, waste water or sewage
- B01D 61/145: {Ultrafiltration}
- B01D 61/147: {Microfiltration}
- B01D 2311/04: Specific process operations in the feed stream; Feed pretreatment
- B01D 2311/26: Further operations combined with membrane separation processes
- B01D 2311/2626: Absorption or adsorption
- B01D 2311/2649: Filtration
- B01D 2317/08: Use of membrane modules of different kinds
- B01D 2325/38: Hydrophobic membranes
- C02F 1/004: {using large scale industrial sized filters}
- C02F 1/26: by extraction
- C02F 1/66: by neutralisation; pH adjustment (for degassing C02F1/20; using ion-exchange C02F1/42; for flocculation or precipitation of suspended impurities C02F1/52; for removing dissolved compounds C02F1/58)
- C02F 5/06: using calcium compounds
- C02F 2101/006: {Radioactive compounds}
- C02F 2101/101: {Sulfur compounds}
- C02F 2101/108: {Boron compounds}
- C02F 2101/301: {Detergents, surfactants}
- C02F 2101/32: Hydrocarbons, e.g. oil
- C02F 2103/08: Seawater, e.g. for desalination
- C02F 2303/22: Eliminating or preventing deposits, scale removal, scale prevention (C02F1/042, C02F1/4602, C02F5/00 take precedence)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)

## Abstract

Conventional oil-water separation methods are inefficient since they break down a given “primary” phase into two “secondary” phases, one is richer and the other one is poorer in the “secondary” phase of the “primary” phase. As such, neither oil is recovered as a readily de-watered stream nor is water recovered as a readily de-oiled stream. However, de-watering and de-oiling of “oil-water” streams are synonymous, and therefore they should be simultaneously targeted by an efficient method. There are provided herein systems and methods to effectively treat “oil-water” streams by simultaneously de-watering the oil phase and de-oiling the water phase, de-scaling the de-oiled water phase, and de-salting the de-scaled water phase.

## Claims

### Claim 1

A method for treating an oil-water stream, said method comprising separating said oil-water stream by a hydrophobic membrane to produce a de-watered oil stream, and a de-oiled water stream; determining that said de-watered oil stream is less than or equal to 10 pounds of salt per thousand barrels of oil (PTB), said de-oiled water stream is less than or equal to 42 mg/L of total oil content (TOC), and combinations thereof; and wherein said oil-water stream is a water-in-oil (W/O) stream, an oil-in-water (O/W) stream, and combinations thereof.

### Claim 2

A method for treating an oil-water stream, said method comprising demulsifying said oil-water stream with a polluting acid gas source, followed with separating by a hydrophobic membrane to produce a de-watered oil stream, a de-oiled water stream, and an acid gas stream; determining that said de-watered oil stream is less than or equal to 10 pounds of salt per thousand barrels of oil (PTB), said de-oiled water stream is less than or equal to 42 mg/L of total oil content (TOC), and combinations thereof; appreciating that said acid gas stream is carbon dioxide, hydrogen sulfide, sulfur dioxide, and combinations thereof; and recognizing that said oil-water stream is a water-in-oil (W/O) stream, an oil-in-water (O/W) stream, and combinations thereof.

### Claim 3 (depends on 2)

The method of claim 2, wherein said polluting acid gas source is selected from the group consisting of emissions from polluting stacks, steam injection facilities for hydrocarbons recovery, and combinations thereof.

### Claim 4 (depends on 2)

The method of claim 2, comprising the step of replacing at least a portion of said polluting acid gas source by the produced said acid gas stream from said hydrophobic membrane.

### Claim 5 (depends on 2)

The method of claim 2, further comprises the step of replacing said polluting acid gas source or at least a portion of said polluting acid gas source with an acid, wherein said acid is selected from the group consisting of hydrochloric acid, perchloric acid, hypochlorous acid, nitric acid, citric acid, sulfuric acid, sulfonic acid, phosphoric acid, formic acid, acetic acid, propionic acid, butyric acid, pentanoic acid, hexanoic acid, pyruvic acid, lactic acid, caproic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, humic acid, fulvic acid, and combinations thereof.

### Claim 6

A method for separating foulants from a de-oiled water stream, said method comprising the steps of: (a) mixing said de-oiled water stream with a calcium source and leonardite to form precipitates comprising said foulants in a pre-precipitator unit; wherein said foulants comprise strontium, barium, radium, naturally occurring radioactive materials (NORM), silica, bromide, boron, transition metals, phosphates, carbonates, sulfides, and combinations thereof; and wherein said calcium source is selected from the group consisting of dolime, calcium oxide, calcium hydroxide, and combinations thereof; and (b) removing said precipitates by a filter to produce a de-fouled water stream.

### Claim 7 (depends on 6)

The method of claim 6, comprising the steps of: (a) separating sulfate from said de-fouled water stream by: (i) mixing said de-fouled water stream with an organic solvent, and aluminum hydroxide or iron hydroxide, to form precipitates comprising calcium sulfoaluminate or calcium sulfoferrate in a precipitator unit; wherein said organic solvent is selected from the group consisting of isopropylamine, propylamine, dipropylamine, diisopropylamine, ethylamine, diethylamine, methylamine, dimethylamine, ammonia, and combinations thereof; (ii) recovering at least a portion of said organic solvent by introducing an inert gas stream into said precipitation unit, wherein said inert gas stream is selected from the group consisting of nitrogen, air, water vapor, and combinations thereof; (iii) filtering said precipitates to produce a de-scaled water stream;
(b) utilizing at least a portion of said de-scaled water stream for hydrocarbons production, hydrocarbons recovery, acid gas scrubbing, and combinations thereof;
and
(c) desalinating at least a portion of said de-scaled water stream by a desalination method to produce a distillate stream and a de-scaled reject brine stream; wherein said desalination method is selected from the group consisting of multi-stage flash desalination, multi-effect distillation, thermal vapor recompression, mechanical vapor recompression, freezing, membrane distillation, vacuum membrane distillation, osmotic membrane distillation, reverse osmosis, nanofiltration, forward osmosis, electrodialysis, pervaporation, and combinations thereof; and wherein said de-scaled reject brine stream is utilized for hydrocarbons production, hydrocarbons recovery, chlor-alkali industries, acid gas scrubbing, production of road de-icing salts, and combinations thereof.

### Claim 8 (depends on 7)

The method of claim 7, further comprises the steps of: (a) feeding at least a portion of said de-scaled water stream to a Recycle-Brine Multi-Stage Flash (RB-MSF) desalination train, wherein said RB-MSF desalination train includes only a heat recovery section, to produce said distillate stream and said de-scaled reject brine; and (b) mixing at least a portion of said de-scaled reject brine with said de-scaled water stream to form a recycle brine stream, and feeding said recycle brine stream to said RB-MSF desalination train to produce said distillate stream and said de-scaled reject brine; wherein a portion of said de-scaled reject brine is discharged from said RB-MSF train at a level not exceeding 250,000 mg/L of total dissolved solids (TDS).

### Claim 9

A method for treating an oil-water stream, said method comprising demulsifying said oil-water stream with an anionated organic solvent, followed by separating by a hydrophobic membrane to produce a de-watered oil stream, a de-oiled water stream, and an acid gas stream; determining that said de-watered oil stream is less than or equal to 10 pounds of salt per thousand barrels of oil (PTB), said de-oiled water stream is less than or equal to 42 mg/L of total oil content (TOC), and combinations thereof; appreciating said acid gas stream is carbon dioxide, hydrogen sulfide, sulfur dioxide, and combinations thereof; and recognizing that said oil-water stream is a water-in-oil (W/O) stream, an oil-in-water (O/W) stream, and combinations thereof.

### Claim 10 (depends on 9)

The method of claim 9, wherein said anionated organic solvent is generated by reacting an organic solvent with acid; wherein said organic solvent is selected from the group consisting of isopropylamine, propylamine, dipropylamine, diisopropylamine, ethylamine, diethylamine, methylamine, dimethylamine, ammonia, and combinations thereof; and wherein said acid is selected from the group consisting of hydrochloric acid, perchloric acid, hypochlorous acid, nitric acid, citric acid, sulfuric acid, sulfonic acid, phosphoric acid, formic acid, acetic acid, propionic acid, butyric acid, pentanoic acid, hexanoic acid, pyruvic acid, lactic acid, caproic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, humic acid, fulvic acid, and combinations thereof.

### Claim 11 (depends on 9)

The method of claim 9, comprising the steps of: (a) separating sulfate from said de-oiled water stream by: (i) mixing said de-oiled water stream with aluminum hydroxide or iron hydroxide to regenerate the organic solvent from said anionated organic solvent, and to form precipitates comprising calcium sulfoaluminate or calcium sulfoferrate in a precipitator unit; (ii) recovering at least a portion of the regenerated said organic solvent by introducing an inert gas stream into said precipitation unit, wherein said inert gas stream is selected from the group consisting of nitrogen, air, water vapor, and combinations thereof; (iii) filtering said precipitates to produce a de-scaled water stream; (iv) reacting the recovered said organic solvent in step (ii) with acid to produce said anionated organic solvent;
(b) utilizing at least a portion of said de-scaled water stream for hydrocarbons production, hydrocarbons recovery, acid gas scrubbing, and combinations thereof; and
(c) desalinating at least a portion of said de-scaled water stream by a desalination method to produce a distillate stream and a de-scaled reject brine stream; wherein said desalination method is selected from the group consisting of multi-stage flash desalination, multi-effect distillation, thermal vapor recompression, mechanical vapor recompression, freezing, membrane distillation, vacuum membrane distillation, osmotic membrane distillation, reverse osmosis, nanofiltration, forward osmosis, electrodialysis, pervaporation, and combinations thereof; and wherein said de-scaled reject brine stream is utilized for hydrocarbons production, hydrocarbons recovery, chlor-alkali industries, acid gas scrubbing, production of road de-icing salts, and combinations thereof.

### Claim 12 (depends on 11)

The method of claim 11, wherein step (a) (i) further comprises the step of mixing said de-oiled water stream with a calcium source; wherein said calcium source is selected from the group consisting of dolime, calcium oxide, calcium hydroxide, and combinations thereof.

### Claim 13 (depends on 11)

The method of claim 11, further comprises the steps of: (a) feeding at least a portion of said de-scaled water stream to a Recycle-Brine Multi-Stage Flash (RB-MSF) desalination train, wherein said RB-MSF desalination train includes only a heat recovery section, to produce said distillate stream and said de-scaled reject brine; and (b) mixing at least a portion of said de-scaled reject brine with said de-scaled water stream to form a recycle brine stream, and feeding said recycle brine stream to said RB-MSF desalination train to produce said distillate stream and said de-scaled reject brine; wherein a portion of said de-scaled reject brine is discharged from said RB-MSF train at a level not exceeding 250,000 mg/L of total dissolved solids (TDS).

### Claim 14

A method for treating an oil-water stream, said method comprising demulsifying said oil-water stream by an aluminum source or an iron source, followed by separating utilizing a hydrophobic membrane to produce a de-watered oil stream, a de-oiled water stream, and an acid gas stream; determining that said de-watered oil stream is less than or equal to 10 pounds of salt per thousand barrels of oil (PTB), said de-oiled water stream is less than or equal to 42 mg/L of total oil content (TOC), and combinations thereof; wherein said acid gas stream comprises carbon dioxide, hydrogen sulfide, sulfur dioxide, and combinations thereof; and wherein said oil-water stream is a water-in-oil (W/O) stream, an oil-in-water (O/W) stream, and combinations thereof.

### Claim 15 (depends on 14)

The method of claim 14, wherein said aluminum source is selected from the group consisting of aluminum chloride, aluminum chlorohydrate, aluminum nitrate, aluminum sulfate, aluminum formate, aluminum acetate, and combinations thereof; and wherein said iron source is selected from the group consisting of iron chloride, iron chlorohydrate, iron nitrate, iron sulfate, iron formate, iron acetate, and combinations thereof.

### Claim 16 (depends on 14)

The method of claim 14, comprising the steps of: (a) separating sulfate from said de-oiled water stream by: (i) mixing said de-oiled water stream with an organic solvent to form precipitates comprising calcium sulfoaluminate or calcium sulfoferrate in a precipitator unit; wherein said organic solvent is selected from the group consisting of isopropylamine, propylamine, dipropylamine, diisopropylamine, ethylamine, diethylamine, methylamine, dimethylamine, ammonia, and combinations thereof; (ii) recovering at least a portion of said organic solvent by introducing an inert gas stream into said precipitation unit, wherein said inert gas stream is selected from the group consisting of nitrogen, air, water vapor, and combinations thereof; (iii) filtering said precipitates to produce a de-scaled water stream;
(b) utilizing at least a portion of said de-scaled water stream for hydrocarbons production, hydrocarbons recovery, acid gas scrubbing, and combinations thereof; and
(c) desalinating at least a portion of said de-scaled water stream by a desalination method to produce a distillate stream and a de-scaled reject brine stream; wherein said desalination method is selected from the group consisting of multi-stage flash desalination, multi-effect distillation, thermal vapor recompression, mechanical vapor recompression, freezing, membrane distillation, vacuum membrane distillation, osmotic membrane distillation, reverse osmosis, nanofiltration, forward osmosis, electrodialysis, pervaporation, and combinations thereof; and wherein said de-scaled reject brine stream is utilized for hydrocarbons production, hydrocarbons recovery, chlor-alkali industries, acid gas scrubbing, production of road de-icing salts, and combinations thereof.

### Claim 17 (depends on 16)

The method of claim 16, wherein step (a) (i) further comprises the step of mixing said de-oiled water stream with a calcium source; wherein said calcium source is selected from the group consisting of dolime, calcium oxide, calcium hydroxide, and combinations thereof.

### Claim 18 (depends on 16)

The method of claim 16, further comprises the steps of: (a) feeding at least a portion of said de-scaled water stream to a Recycle-Brine Multi-Stage Flash (RB-MSF) desalination train, wherein said RB-MSF desalination train includes only a heat recovery section, to produce said distillate stream and said de-scaled reject brine; and (b) mixing at least a portion of said de-scaled reject brine with said de-scaled water stream to form a recycle brine stream, and feeding said recycle brine stream to said RB-MSF desalination train to produce said distillate stream and said de-scaled reject brine; wherein a portion of said de-scaled reject brine is discharged from said RB-MSF train at a level not exceeding 250,000 mg/L of total dissolved solids (TDS).