US3764517A - Solvent dewaxing process - Google Patents

Solvent dewaxing process Download PDF

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Publication number
US3764517A
US3764517A US00100070A US3764517DA US3764517A US 3764517 A US3764517 A US 3764517A US 00100070 A US00100070 A US 00100070A US 3764517D A US3764517D A US 3764517DA US 3764517 A US3764517 A US 3764517A
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United States
Prior art keywords
solvent
oil
wax
temperature
filtration
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Expired - Lifetime
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US00100070A
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English (en)
Inventor
R Bodemuller
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Texaco Inc
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Texaco Inc
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/02—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils
    • C10G73/06—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils with the use of solvents

Definitions

  • Wax and dewaxed oils are recovered as products and solvent is recovered for recycle and reuse in the US. Cl. process olvent is added to the heated wax- [51] Int. Cl. (210g 43/08 bearing il to rapidly cool the oil-solvent mixture to a [58] Field of Search 208/33 temperature below the temperature of the melting point of the wax contained therein and above the tem- References Cited perature at which wax is crystallized from the oil- UNITED STATES PATENTS solvent mixture. The cooled oil-solvent mixture is then 3,549,514 12/1970 Brown et al.
  • 208/33 chilled at a final chilling rate of Per 3,642,609 2/1972 Mayer et a] r 208/33 to a filtration temperature above 10 below the pour 2,410,483 11/1946 Dons et a] 208/33 p int f th dewaxed i pr
  • the filtration rate is Primary Examinerl-lelen M. S. Sneed Attorney-Thomas l-l. Whaley and Carl G. Reis continuously determined and the final chilling rate is controlled in response thereto.
  • the waxy oil and solvent are customarily mixed and the mixture heated to a temperature sufficien't to effect complete solution of the waxy oil and solvent. It is known that the dewaxing filtration rate may be substantially increased by heating the mixture of waxy oil and solvent to a temperature of l to 50F. above the minimum temperature of complete solution prior to beginning chilling as is described in Knowles U.S. Pat. No. 2,137,209.
  • the wax melting point will depend upon the particular stock treated and may vary, for example, from about 100F. for the wax separated from a light paraffinic lubrication stock such as a spindle distillate to about 210F. for the wax separated from a deasphalted residual stock such as bright stock.
  • Solvent is then added in any suitable manner to the preheated wax-bearing oil.
  • the solvent employed is at a relatively low temperature within the range of about 60 to 135F. affecting equilibration of the temperature of the oil-solvent mixture to a temperature within the range of about 80 to 150F.
  • the oilsolvent mixture is then cooled by indirect heat exchange to a temperature of 0 to F. below the pour point of the desired oil product by indirect heat exchange. Further dilution with solvent in the course of chilling may also be effected.
  • Chilling by dilution of the preheated oil charge with cold solvent is effected substantially instantaneously, i.e., within the period of about 5 to seconds required for complete mixing.
  • shock chilling at an actual rate of about 100 to 1,000F. per minute is readily obtained.
  • chilling at a rate of 0.3" to F. per minute is typically employed and is readily obtainable in scraped wall double pipe heat exchangers. Accordingly, it is an object of this invention to provide an improved dewaxing process. Another object of the invention is to provide an improved process for the dewaxing of waxy lubricating oils.
  • Still another object of this invention is to provide a method for increasing the dewaxing capacity of a dewaxing plant such as a plant for the dewaxing of waxy mineral oils or for the solvent fractional crystallization or separation of waxes from mineral oils, fatty acids, vegetable oils, animal oils and fish oils.
  • An advantage of the process of this invention is that dewaxing may be effected at higher throughputs than heretofore obtainable while maintaining high yields of dewaxed oil and low oil content of the separated wax. It has been found that the use of the method of this invention has resulted in increases of 10 to 30 percent in the throughput capacity of a given dewaxing facility and uniformly high throughputs are obtained with variation in solvent compositions.
  • Oil charge for example, a wax-bearing mineral oil separated by vacuum distillation of a paraffin base crude oil is introduced as charge through line 1 into heater 2.
  • Heater 2 may be a shell and tube type heat exchanger heated with steam or a hot heat transfer fluid passed through coil 3 or advantageously may comprise the charge oil storage tankage heated by means of immersed steam coils.
  • the oil charge is heated in heater 2 to a temperature of at least the melting point of the wax contained in the charge and preferably to a temperature 5 to F. above the melting point of the wax contained in the charge oil.
  • Chiller 12 is desirably a scraped wall double pipe heat exchanger. It is necessary to provide means to scrape the walls of chiller 12 since the precipitated wax would otherwise deposit on the cooling surface and reduce the efficiency of the heat exchange. Cooling is effected by heat exchange with ammonia, evaporating propane, brine or other means of refrigeration well known in the art.
  • Filtrate from the repulp filtration from line 13 is introduced as secondary dilution at an intermediate point in chiller 12.
  • the filtrate in line 13 is predominantly solvent and is at the low temperature of the repulp filtration.
  • Slurry of wax particles in cold solvent-oil mixture is discharged from chiller 12 through line 15 to primary filter 16.
  • primary filter l6 wax is separated by filtration from primary filtrate comprising dewaxed oil and solvent.
  • the dewaxed oil and solvent is discharged through line 17.
  • Filter cake in primary filter 16 is cold washed with solvent introduced through line 18 and the resulting filter cake is discharged through line 19.
  • the primary filter cake is repulped by dilution with additional solvent from line 21 and the resulting slurry of wax in solvent is passed to repulp filter 23.
  • repulp filter 23 occluded oil is washed from the wax particles and the resulting filtrate is discharged through line 13 for recycle back to chiller 12.
  • the separated wax in repulp filter 23 is cold washed with solvent from line 25 and the washed wax is then passed through line 26 to solvent stripper 27.
  • solvent stripper 27 solvent is distilled from the wax and product wax is discharged through line 28. Recovered solvent is discharged through line 29 for recycle and reuse in the process.
  • the solvent used in the solvent dewaxing process is of a selective type having a substantially complete solvent action upon the oil component of the waxy oil charge, and substantially no solvent action upon the wax contained therein at dewaxing temperatures of about 10 to -30F.
  • a solvent comprises, for example, a mixture of an aliphatic ketone, such as acetone, methyl ethyl ketone or methyl isobutyl ketone and an aromatic hydrocarbon such as benzene, tolu ene, or a mixture of benzene and toluene. It is contemplated, however, that mixtures of other aliphatic ketones and aromatic hydrocarbons may be employed, or that aromatic hydrocarbons may be employed by themselves.
  • Such solvents as low boiling petroleum hydrocarbons including naphtha, gasoline, pentane, or mixtures thereof may be used as may certain hydrocarbon derivatives such as dichloromethane, methylene chloride, chloroform, and ethers.
  • This invention is particularly adapted to the dewaxing of wax-bearing mineral oil derived from paraffin base crude, examples of which include Pennsylvania, East Texas, Rhodesia, paraffinic Venezuelan, and so forth. Such crudes contain about 5 to 50 percent of wax by volume of the oil.
  • the temperature of the solvent in line 9 is controlled to control the temperature of the oil-solvent mixture passed to chiller 12. Control of this mixture temperature while maintaining a constant chiller outlet temperature provides a means of controlling the differential temperature across chiller 12 and hence means for controlling the cooling rate.
  • the filtration rate is maximized by measuring the rate of flow of the filtrate in line 17 by rate of flow meter 40. Rate of flow meter 40 generates a signal representative of the filtration rate.
  • the temperature of the solvent in line 9 is determined by temperature meter controller 41 which controls coolant in line 42 passed to cooler 43. Temperature meter controller 41 is reset by the signal from rate of flow meter 40 to optimize the filtration rate.
  • Optimization is effected with a logic circuit providing a directional signal which includes conventional analog-todigital converters, shift registers, digital-to-analog converters and a comparator whose arrangements are straight forward and the details of which are not necessary for the understanding of the inventions by one skilled in the art.
  • a lubricating oil stock containing wax having a melting point of I52F. was solvent dewaxed in a comparative test in which three consecutive tests, A, B, and C were made.
  • a and C the oil was heated to a temperature above the melting point of the wax contained in the charge prior to dilution with solvent and chilling.
  • Test B the charge was heated to a temperature above the cloud and pour point of the charge stock but below the melting point of the wax contained therein prior to dilution with solvent and chilling.
  • a process for the separation of wax from a waxbearing oil which comprises separately heating the wax-bearing oil to a temperature above the melting point of the wax contained therein, shock-chilling the heated oil at a rate between 100F. and 1,000F. per minute to a temperature between 80F. and F. by the addition of solvent thereto, chilling the resulting oil-solvent mixture at a rate between 0.3F. and 3.0F. per minute by indirect heat exchange to a temperature between 0F. and 15F.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)
US00100070A 1970-12-21 1970-12-21 Solvent dewaxing process Expired - Lifetime US3764517A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US10007070A 1970-12-21 1970-12-21

Publications (1)

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US3764517A true US3764517A (en) 1973-10-09

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Application Number Title Priority Date Filing Date
US00100070A Expired - Lifetime US3764517A (en) 1970-12-21 1970-12-21 Solvent dewaxing process

Country Status (22)

Country Link
US (1) US3764517A (de)
JP (1) JPS503763B1 (de)
AR (1) AR212231A1 (de)
AT (1) AT341637B (de)
AU (1) AU451794B2 (de)
BE (1) BE775817A (de)
BR (1) BR7107984D0 (de)
CA (1) CA952845A (de)
DE (1) DE2131844A1 (de)
DK (1) DK134566B (de)
EG (1) EG10531A (de)
ES (1) ES397236A1 (de)
FI (1) FI55518B (de)
FR (1) FR2118914B1 (de)
GB (1) GB1326326A (de)
IT (1) IT944223B (de)
NL (1) NL166055C (de)
PH (1) PH9605A (de)
SE (1) SE376630B (de)
TR (1) TR17836A (de)
YU (1) YU35160B (de)
ZA (1) ZA717553B (de)

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4115245A (en) * 1977-07-05 1978-09-19 Texaco Inc. Solvent dewaxing process
US4115242A (en) * 1977-07-05 1978-09-19 Texaco Inc. Solvent dewaxing process
US4115241A (en) * 1977-07-05 1978-09-19 Texaco Inc. Solvent dewaxing process
US4128472A (en) * 1977-07-05 1978-12-05 Texaco Inc. Solvent dewaxing process
FR2413463A1 (fr) * 1977-12-27 1979-07-27 Exxon Research Engineering Co Procede pour le deparaffinage d'huile de recuperation
WO1982000029A1 (en) * 1980-06-20 1982-01-07 Pitman H Solvent dewaxing process
US4354921A (en) * 1981-07-27 1982-10-19 Texaco Inc. Solvent dewaxing process
US4444648A (en) * 1982-03-08 1984-04-24 Exxon Research And Engineering Co. Solvent dewaxing with methyl tertiary butyl ether
EP0348044A2 (de) * 1988-06-20 1989-12-27 Texaco Development Corporation Kontrollanlage für das Entparaffinieren von Schmierölen mit Lösungsmitteln
US5474668A (en) * 1991-02-11 1995-12-12 University Of Arkansas Petroleum-wax separation
US5853564A (en) * 1991-02-11 1998-12-29 University Of Arkansas Petroleum-wax separation
US20060030499A1 (en) * 1996-06-18 2006-02-09 Oommen Thottathil V Electrical transformer with vegetable oil dielectric fluid
WO2006096872A2 (en) * 2005-03-09 2006-09-14 Cargill, Incorporated Separation of sunflower oil and wax
WO2009051495A1 (en) * 2007-10-19 2009-04-23 Statoilhydro Asa Method for wax removal and measurement of wax thickness
US20100065469A1 (en) * 2006-10-23 2010-03-18 Palmer Thomas R Method for on-line monitoring of wax crystallization

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5213944U (de) * 1975-07-18 1977-01-31

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2410483A (en) * 1944-11-13 1946-11-05 Mid Continent Petroleum Corp Processes of dewaxing oils
US3549514A (en) * 1969-01-09 1970-12-22 Texaco Inc Methods and apparatus for monitoring and control of solvent dewaxing processes
US3642609A (en) * 1969-11-13 1972-02-15 Exxon Research Engineering Co Dewaxing waxy oil by dilution chilling

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2410483A (en) * 1944-11-13 1946-11-05 Mid Continent Petroleum Corp Processes of dewaxing oils
US3549514A (en) * 1969-01-09 1970-12-22 Texaco Inc Methods and apparatus for monitoring and control of solvent dewaxing processes
US3642609A (en) * 1969-11-13 1972-02-15 Exxon Research Engineering Co Dewaxing waxy oil by dilution chilling

Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4115245A (en) * 1977-07-05 1978-09-19 Texaco Inc. Solvent dewaxing process
US4115242A (en) * 1977-07-05 1978-09-19 Texaco Inc. Solvent dewaxing process
US4115241A (en) * 1977-07-05 1978-09-19 Texaco Inc. Solvent dewaxing process
US4128472A (en) * 1977-07-05 1978-12-05 Texaco Inc. Solvent dewaxing process
FR2413463A1 (fr) * 1977-12-27 1979-07-27 Exxon Research Engineering Co Procede pour le deparaffinage d'huile de recuperation
US4169039A (en) * 1977-12-27 1979-09-25 Exxon Research & Engineering Co. Recovering useful oil from wax filter hot washings and dumped slurry
WO1982000029A1 (en) * 1980-06-20 1982-01-07 Pitman H Solvent dewaxing process
US4354921A (en) * 1981-07-27 1982-10-19 Texaco Inc. Solvent dewaxing process
US4444648A (en) * 1982-03-08 1984-04-24 Exxon Research And Engineering Co. Solvent dewaxing with methyl tertiary butyl ether
EP0348044A2 (de) * 1988-06-20 1989-12-27 Texaco Development Corporation Kontrollanlage für das Entparaffinieren von Schmierölen mit Lösungsmitteln
EP0348044A3 (en) * 1988-06-20 1990-02-21 Texaco Development Corporation Lube oil solvent dewaxing control system
US5474668A (en) * 1991-02-11 1995-12-12 University Of Arkansas Petroleum-wax separation
US5853564A (en) * 1991-02-11 1998-12-29 University Of Arkansas Petroleum-wax separation
US6024862A (en) * 1991-02-11 2000-02-15 Advanced Refining Technologies, Inc. Petroleum-wax separation
US20060030499A1 (en) * 1996-06-18 2006-02-09 Oommen Thottathil V Electrical transformer with vegetable oil dielectric fluid
WO2006096872A2 (en) * 2005-03-09 2006-09-14 Cargill, Incorporated Separation of sunflower oil and wax
WO2006096872A3 (en) * 2005-03-09 2007-08-02 Cargill Inc Separation of sunflower oil and wax
US8029661B2 (en) * 2006-10-23 2011-10-04 Exxonmobil Research And Engineering Company Method for on-line monitoring of wax crystallization
US20100065469A1 (en) * 2006-10-23 2010-03-18 Palmer Thomas R Method for on-line monitoring of wax crystallization
US20100300486A1 (en) * 2007-10-19 2010-12-02 Statoil Asa Method for wax removal and measurement of wax thickness
CN101896688A (zh) * 2007-10-19 2010-11-24 斯塔特伊公司 清除蜡和测量蜡厚度的方法
GB2468220A (en) * 2007-10-19 2010-09-01 Statoil Asa Method for wax removal and measurement of wax thickness
WO2009051495A1 (en) * 2007-10-19 2009-04-23 Statoilhydro Asa Method for wax removal and measurement of wax thickness
GB2468220B (en) * 2007-10-19 2012-06-06 Statoil Asa Method for wax removal and measurement of wax thickness
EA018505B1 (ru) * 2007-10-19 2013-08-30 Статойл Аса Способ удаления парафина и измерения толщины парафина
US8623147B2 (en) 2007-10-19 2014-01-07 Statoil Petroleum As Method for wax removal and measurement of wax thickness
CN101896688B (zh) * 2007-10-19 2014-07-23 斯塔特伊石油公司 清除蜡和测量蜡厚度的方法
EA022677B1 (ru) * 2007-10-19 2016-02-29 Статойл Аса Способ и устройство для измерения толщины отложений парафина в трубе или перерабатывающем оборудовании
EA022677B8 (ru) * 2007-10-19 2020-03-19 Статойл Аса Способ и устройство для измерения толщины отложений парафина в трубе или перерабатывающем оборудовании
EA018505B8 (ru) * 2007-10-19 2020-03-27 Статойл Петролеум Ас Способ удаления парафина и измерения толщины парафина

Also Published As

Publication number Publication date
BE775817A (fr) 1972-05-25
SE376630B (sv) 1975-06-02
DE2131844A1 (de) 1972-07-13
GB1326326A (en) 1973-08-08
YU295371A (en) 1980-03-15
AT341637B (de) 1978-02-27
BR7107984D0 (pt) 1973-04-10
FI55518B (fi) 1979-04-30
NL166055B (nl) 1981-01-15
AU3580271A (en) 1973-05-24
TR17836A (tr) 1976-04-13
CA952845A (en) 1974-08-13
NL166055C (nl) 1981-06-15
DK134566C (de) 1977-05-09
NL7117434A (de) 1972-06-23
IT944223B (it) 1973-04-20
JPS503763B1 (de) 1975-02-10
PH9605A (en) 1976-01-19
FR2118914B1 (de) 1976-03-26
ATA720871A (de) 1977-06-15
FR2118914A1 (de) 1972-08-04
DK134566B (da) 1976-11-29
EG10531A (en) 1983-12-31
YU35160B (en) 1980-09-25
AU451794B2 (en) 1974-07-18
AR212231A1 (es) 1978-06-15
ZA717553B (en) 1973-03-28
ES397236A1 (es) 1974-05-01

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