# US 6,106,699 A · Process for de-chlorinating and de-fouling oil

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- Number: US 6,106,699 A
- Document ID: US6106699A
- Status: Granted
- Kind: A
- Application number: 09/067,031
- Filed: 1998-04-28
- Granted: 2000-08-22
- Earliest claimed: 1998-04-28
- Assignees: ProbeX Inc.
- Inventors: Martin R. MacDonald; Alexander D.B. Daspit; Thomas G. Murray
- Web page: https://patentgrep.com/patent/US6106699A

## CPC

- C02F 1/048: {Purification of waste water by evaporation}
- C10G 31/06: by heating, cooling, or pressure treatment
- C10M 175/00: Working-up used lubricants to recover useful products {(destructive distillation C10B; extraction and elimination of PCBs C10G7/006, C10G21/006, C10G25/006; combustion processes F23G; filtration, filters in general B01D); Cleaning (in a mechanical way B08B; integrated processes C23; solid waste B09B)}
- C10M 175/0025: {by thermal processes}
- C10M 175/0033: {using distillation processes; devices therefor}
- C10M 175/02: mineral-oil based
- 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)
- 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
- C10M: LUBRICATING COMPOSITIONS (well drilling compositions C09K8/02); USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION (mould release, i.e. separating, agents for metals B22C3/00, for plastics or substances in a plastic state, in general B29C33/56, for glass C03B40/02; textile lubricating compositions D06M11/00, D06M13/00, D06M15/00; immersion oils for microscopy G02B21/33)

## Abstract

The invention is directed to a process of reducing the chlorine content of oil as well as its propensity to foul during subsequent distillation processes. The process heats the oil to a temperature in the range of 400 to 700 F and contacts the oil with a non-oxidizing gas, such as steam, for a residence time of at least several minutes. Thereafter the oil may be distilled and/or finished to a base lubricating oil or other distillate product. The oil subject to the process may be used oil, and can be subject to a dewatering or removal of light contaminants treatment prior to being subject to the process.

## Claims

### Claim 1

A method for reducing the propensity of oil to foul, comprising the steps of
heating a quantity of said oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said oil within said temperature range for an average residence time of no less than several minutes
contacting said heated oil with a substantially non-oxidizing gas during said residence time.

### Claim 2 (depends on 1)

A method as in claim 1 wherein the oil is a used oil.

### Claim 3 (depends on 2)

A method as in claim 2 comprising the additional step of:
reducing oil portions carried overhead by said contacting step.

### Claim 4 (depends on 3)

A method as in claim 3 wherein said reducing step is performed by operating said method at a pressure exceeding approximately 5 psig above atmospheric pressure.

### Claim 5 (depends on 3)

A method as in claim 3 wherein said reducing step is accomplished using a contactor through which said oil portions carried overhead are passed.

### Claim 6 (depends on 3)

A method as in claim 3 comprising the additional step of:
condensing said overhead oil portions using a direct contact condenser.

### Claim 7 (depends on 2)

A method as in claim 2 comprising the additional step of:
removing substantially all water and light fuel, having a boiling point below about 300 F at atmospheric pressure, at least a portion of any commercial solvent, and of glycol contamination prior to said heating step.

### Claim 8 (depends on 7)

A method as in claim 7 wherein said removing step is accomplished using a distillation process.

### Claim 9 (depends on 8)

A method as in claim 8 comprising the additional step of:
burning a substantial portion of said water, light fuel, commercial solvents, and glycols for energy recovery without condensation.

### Claim 10 (depends on 2)

A method as in claim 2 comprising the additional step of:
removing substantially all water from said quantity of oil prior to said heating step using a distillation process,
burning a substantial portion of said water and any fuel removed therewith, without condensation.

### Claim 11 (depends on 2)

A method as in claim 2 comprising the additional step of:
maintaining a condensable oil component of oil portions carried overhead by said contacting step at a temperature above approximately 400 F for a period of time exceeding several minutes at higher than atmospheric pressure.

### Claim 12 (depends on 2)

A method as in claim 2 comprising the additional step of:
returning a condensable component of oil portions carried overhead by said contacting step into said quantity of heated oil.

### Claim 13 (depends on 2)

A method as in claim 2 comprising the additional step of:
vacuum distilling said quantity of oil following said contacting step in a vacuum column to produce at least one distillate fraction and a heavier residue.

### Claim 14 (depends on 13)

A method as in claim 13 wherein said vacuum distilling step occurs with an absolute flash zone pressure of at least approximately 10 mm Hg.

### Claim 15 (depends on 13)

A method as in claim 13 wherein a partial pressure of said oil is reduced below its absolute pressure during said vacuum distilling step.

### Claim 16 (depends on 13)

A method as in claim 13 comprising the additional step of:
finishing a portion of said at least one distillate fraction to a base oil using a solvent extraction process.

### Claim 17 (depends on 1)

A method as in claim 1 wherein the contacting gas is substantially comprised of steam.

### Claim 18 (depends on 2)

A method as in claim 2 wherein the contacting gas is substantially comprised of steam.

### Claim 19 (depends on 18)

A method as in claim 18 comprising the additional step of:
condensing a portion of said steam for reuse.

### Claim 20 (depends on 2)

A method as in claim 2 comprising the additional step of:
breaking up bubbles in said quantity of oil from said gas contacting step.

### Claim 21 (depends on 20)

A method as in claim 20 wherein said breaking step is performed using physical agitation of at least a portion of said quantity of oil.

### Claim 22 (depends on 20)

A method as in claim 20 wherein said breaking step is performed using the application of sonic energy to at least a portion of said quantity of oil.

### Claim 23 (depends on 2)

A method as in claim 2, comprising the additional step of:
agitating at least a portion of said quantity of oil.

### Claim 24

A method for reducing the chlorine content of chlorinated oil, comprising the steps of:
heating a quantity of said oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated oil with steam during said residence time.

### Claim 25

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time.

### Claim 26

A method for reducing the propensity of used oil to foul, comprising the steps of:
removing from a quantity of said used oil substantially all water and light fuel, having a boiling point below about 300 F at atmospheric pressure, and at least a portion of any commercial solvent, and glycol contamination,
heating said quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said quantity of said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said quantity of used oil with a substantially non-oxidizing gas during said residence time.

### Claim 27

A method for reducing the propensity of used oil to foul, comprising the steps of:
removing substantially all water from a quantity of said used oil using a distillation process,
burning a substantial portion of said water and any fuel removed therewith, without condensation,
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated oil with a substantially non-oxidizing gas during said residence time.

### Claim 28

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
vacuum distilling at least a portion of said quantity of used oil in a vacuum column to produce at least one distillate fraction and a heavier residue.

### Claim 29

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
vacuum distilling at least a portion of said quantity of used oil in a vacuum column to produce at least one distillate fraction and a heavier residue, wherein a partial pressure of said used oil is reduced below its absolute pressure during said vacuum distilling step.

### Claim 30

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
vacuum distilling at least a portion of said quantity of used oil in a vacuum column to produce at least one distillate fraction and a heavier residue,
finishing at least a portion of said at least one distillate fraction to a base oil using a solvent extraction process.

### Claim 31

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
breaking up bubbles in said used oil during said gas contacting step.

### Claim 32

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than several minutes, wherein at least two sequential reactors accomplish said step of maintaining,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time.

### Claim 33 (depends on 32)

A method as in claim 32, wherein at least two sequential reactors accomplish said step of contacting.

### Claim 34

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time.

### Claim 35

A method for reducing the propensity of used oil to foul, comprising the steps of:
removing from a quantity of said used oil substantially all water and light fuel, having a boiling point below about 300 F at atmospheric pressure, and at least a portion of any commercial solvent, and glycol contamination,
heating said quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said quantity of said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said quantity of used oil with a substantially non-oxidizing gas during said residence time.

### Claim 36

A method for reducing the propensity of used oil to foul, comprising the steps of:
removing substantially all water from a quantity of said used oil using a distillation process,
burning a substantial portion of said water and any fuel removed therewith, without condensation,
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said heated oil with a substantially non-oxidizing gas during said residence time.

### Claim 37

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
vacuum distilling at least a portion of said quantity of used oil in a vacuum column to produce at least one distillate fraction and a heavier residue.

### Claim 38

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
vacuum distilling at least a portion of said quantity of used oil in a vacuum column to produce at least one distillate fraction and a heavier residue, wherein a partial pressure of said used oil is reduced below its absolute pressure during said vacuum distilling step.

### Claim 39

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
vacuum distilling at least a portion of said quantity of used oil in a vacuum column to produce at least one distillate fraction and a heavier residue,
finishing at least a portion of said at least one distillate fraction to a base oil using a solvent extraction process.

### Claim 40

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time,
breaking up bubbles in said used oil during said gas contacting step.

### Claim 41

A method for reducing the propensity of used oil to foul, comprising the steps of:
heating a quantity of said used oil to a temperature in the range of approximately 400 F to 700 F,
maintaining said used oil within said temperature range for an average residence time of no less than fifteen minutes, wherein at least two sequential reactors accomplish said step of maintaining,
contacting said heated used oil with a substantially non-oxidizing gas during said residence time.

### Claim 42 (depends on 41)

A method as in claim 41, wherein at least two sequential reactors accomplish said step of contacting.
