US3259549A - Process for improving cloud point of petroleum gas oil by caustic washing thereof from hydrocarbon mixtures - Google Patents

Process for improving cloud point of petroleum gas oil by caustic washing thereof from hydrocarbon mixtures Download PDF

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Publication number
US3259549A
US3259549A US330526A US33052663A US3259549A US 3259549 A US3259549 A US 3259549A US 330526 A US330526 A US 330526A US 33052663 A US33052663 A US 33052663A US 3259549 A US3259549 A US 3259549A
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Prior art keywords
organism
oil
gas oil
yeast
micro
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US330526A
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English (en)
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Vernet Charles
Laine Bernard Maurice
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BP PLC
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BP PLC
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Classifications

    • 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
    • C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/12—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one alkaline treatment step
    • 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
    • C10G32/00—Refining of hydrocarbon oils by electric or magnetic means, by irradiation, or by using microorganisms
    • 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
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
    • C10G67/14—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only including at least two different refining steps in the absence of hydrogen
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/8215—Microorganisms
    • Y10S435/822—Microorganisms using bacteria or actinomycetales
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/8215—Microorganisms
    • Y10S435/911—Microorganisms using fungi
    • Y10S435/921—Candida
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/8215—Microorganisms
    • Y10S435/911—Microorganisms using fungi
    • Y10S435/921—Candida
    • Y10S435/923—Candida lipolytica
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/8215—Microorganisms
    • Y10S435/911—Microorganisms using fungi
    • Y10S435/944—Torulopsis

Definitions

  • pertoleum fractions particularly gas oils
  • the wax is removed by precipitation 'by means of solvents, the wax originally present in the fraction being recovered as such, that is, without conversion to more valuable products.
  • the petroleum fractions boiling below the gas oils for example, heavy naphthenes and kerosines also contain straight chain hydrocarbons which are potentially valuable for conversion to other products but hitherto, in general, utilisation of these hydrocarbons has been rendered difficult by the necessity of recovering these hydrocarbons from the petroleum fractions, in which they are contained, before they can be converted to other products.
  • a process which comprises, in a micro-organism growth stage, cultivating a micro-organism in the presence of a hydrocarbon feedstock consisting of a mixture of straight chain hydrocarbons with other hydrocarbons; in the presence of an aqueous nutrient medium; and in the presence of gas containing free oxygen, thereafter separating the micro-organism from the hydrocarbon residue and subjecting this residue to a caustic wash.
  • feedstock a hydrocarbon fraction derived from petroleum.
  • the process of the invention is of particular value for the treatment of petroleum gas oil fractions which contain straight-chain hydrocarbons in the form of waxes, since by the process of the invention, a gas oil of improved pour point is obtained while the waxes are converted to a valuable product.
  • straight-chain hydrocarbons will be present in the feedstocks according to the invention as paraffins; however, the straight chain hydrocarbons may be present as olefins; also there may be used a mixture containing straight chain parafiins and olefins.
  • the percentage conversion of straight chain hydrocarbons which is achieved can be maintained at a value approaching without necessitating a very disproportionate expenditure of contact time to achieve small improvements. Furthermore, in the continuous process, this high percentage conversion can be achieved without resorting to the use of a long reaction path.
  • Suitable feedstocks to the process of the invention include kerosine, gas oils and lubricating oils; these feedstocks may be unrefined or may have undergone some refinery treatment, but will usually be required to contain a proportion of straight chain hydrocarbons in order to fulfil the purpose of this invention.
  • the petrol- .eum fraction will contain 3-45 by weight of straight chain hydrocarbons.
  • Micro-organisms which are cultivated as herein described may be yeasts, moulds or bacteria.
  • a yeast is employed this is of the family C-ryptococcaceae and particularly of the subafamily Cryptococcoideae; however, if desired there may be used, for example, ascosporogeneous yeasts of the sub-family Saccharomycoideae.
  • Preferred genera of the Cryptococcoideae sub-family are Torulops-is (also known as Torula) and Candida.
  • Preferred strains of yeast are as follows. In particular it is preferred to use the specific stock of indicated Baarn reference numbers; these reference numbers refer to stock held by the Centraal Bureau vor Schi'mmelculture, Baarn, Holland:
  • Candida lipolytica Candida pulcherrima CBS 610 Candida utilis Candida utilis, variati major, CBS 841 Candida tropicalis, CBS 2317 T ornlopsz's collisculosa, CBS 133 Hansenula anomala, CBS Oidium lactis Neurospora sitophila Of the above Candida lipolytica is particularly preferred.
  • the micro-organism may be a mould.
  • a suitable strain is Penicillium expansum.
  • the micro-organism may be a bacterium.
  • the bacteria are of one of the orders: Pseudomonadales, Eubacteriale-s and Actinomycetales.
  • the bacteria which are employed are of the family Bacillaceae and Pseudomonadaceae.
  • Preferred species are Bacillus megaterium, Bacillus subtilis and Pseudomonas aeruginosa.
  • Other strains which may be employed include:
  • Suitable moulds are of the family Aspergillaceae.
  • a suitable genus is Penicillium.
  • Penicillium exparzsum is Aspergillus.
  • cultivation is carried out in the presence of an aqueous nutrient medium.
  • an aqueous nutrient medium may be employed.
  • certain solid nutrient media may be employed.
  • Penicillizrm expansum is suitable for cultivation in an aqueous nutrient medium containing hydrocarbons.
  • Penicillium roqueforti Penicillz'um notatum, Aspargillus fussigatus and Aspergillus niger, Aspergillus versicolor may be used for cultivation on a solid agent containing hydrocarbons as feedstock.
  • an aqueous nutrient medium and a supply of oxygen preferably in the form of air.
  • a typical nutrient medium for the growth of Nocardia a genus in the Actinomycetales order, has the following composition:
  • a suitable nutrient medium has the composition:
  • Yeast extract grams 0.025 (Made up to 1000 mls. with distilled water.)
  • a suitable nutrient medium for yeasts (and moulds) has the composition:
  • the growth of the micro-organism used is favoured by the addition to the culture medium of a very small proportion of extract of yeast (an industrial product rich in vitamins of group B obtained by the hydrolysis of a yeast) or more generally of vitamins of group B and/or biotin.
  • This quantity is preferably of the order of 25 parts per million with reference to the aqueous fermentation medium. It can be higher or lower according to the conditions chosen for the growth.
  • the growth of the micro-organism takes place at the expense of the feedstock fraction with the intermediate production of bodies having an acid function, principally fatty acids, in such manner that the pH of the aqueous mineral medium progressively diminishes. If one does not correct it the growth is fairly rapidly arrested and the concentration of the micro-organism in the medium, that is cellular density no longer increases so that there is reached a so-called stationary phase.
  • the aqueous nutrient medium is maintained at a desired pH by the step-wise or continuous addition of an aqueous medium of high pH value.
  • an aqueous medium of high pH value usually, when using moulds or yeasts and in particular when using Candida lipolytica, the pH of the nutrient medium will be maintained in the range 3-6 and preferably in the range 4-5. (Bacteria require a higher pH, usually 6.58.)
  • Suitable alkaline materials for addition to the growth mixture include sodium hydroxide, potassium hydroxide, disodium hydrogen phosphate and ammonia, either free or in aqueous solution.
  • the optimum temperature of the growth mixture will vary according to the types of micro-organism employed and will usually lie in the range 25-35 C. When using Candida lipolytica the preferred temperature range is 28-32" C.
  • the take-up of oxygen is essential for the growth of the micro-organism.
  • the oxygen will usually be provided as air.
  • the air, used to provide oxygen should be present in the form of fine bubbles under the action of stirring.
  • the air may be introduced through a sintered surface. However there may be used the system of intimate aeration known as vortex aeration.
  • the micro-organism will usually grow initially at a low rate of increase in cellular density. (This period of growth is referred to as the lag phase) Subsequently the rate of growth will increase to a higher rate of growth; the period at the higher rate of growth is referred to as the exponential phase and subsequently again the cellular density will become constant (the stationary phase).
  • a supply of the micro-organism for starting the next batch will preferably be removed before the termination of the exponential phase.
  • the growth operation will usually be discontinued before the stationary phase.
  • the micro-organism will usually be separated from the bulk of the aqueous nutrient medium and from the bulk of the unused feedstock fraction.
  • micro-organism may be subjected to autolysis before further purification of the product.
  • the major part of the continuous aqueous phase is first separated; preferably this is carried out by centrifuging or decanting.
  • the separated aqueous phase will usually contain a greater concentration of non-nutritive ions than can be tolerated in the recycle stream and when this is so, only a portion of the recovered aqueous phase can be recycled.
  • the recycle stream is supplied with make-up quantities of the necessary nutrients and is returned to the fermenter; if desired the make-up materials may be fed to the fermenter as a separate stream.
  • the process as applied to the cultivation of a yeast, may incorporate product separation stages as follows. In some cases micro-organisms other than yeasts may be separated in this manner. I
  • a yeast cream consisting of yeast, having a quantity of oil fixed onto the cells, together with aqueous phase.
  • fraction (ii) fraction (iii) or a blend of fractions (i) and (iii) is mixed with an aqueous solution of a surfactant.
  • the purpose of this treatment is to separate the oil from the yeast cells; the oil being apparently held to the cells by adsorption.
  • an edible surfactant for example a saccharose ester, which makes it possible to reduce the subsequent washing required to remove from the yeast a surfactant which is not edible.
  • the emulsion so formed is broken down by centrifuging to obtain three fractions.
  • a yeast cream consisting of yeast still contaminated by oil together with an aqueous surfactant phase.
  • the aqueous washing solution containing it is recycled.
  • Fraction (vi) may be further treated by alternate washing with surfactant and centrifuging until the oil content of the yeast has reached a desired low value.
  • the yeast cream now consisting of yeast and aqueous surfactant may now be washed with water and again centrifuged. If desired two or more washings may be given to this yeast cream. If desired, one or more of these water washings (but preferably not the last) may make use of salt water (for example, sea water); preferably the final wash is with soft water.
  • the whole of this water coming from the last washing is employed for making up the nutritive medium for the fermentation, where necessary at the stage of washing with the solution of surfactant, and the rest is sent to the salt water used for washing with a view to reducing its salt concentration.
  • the yeast may be dried under conditions suitable for its subsequent use as a foodstuff.
  • the recovered unmetabolised hydrocarbon with or without an intervening refining stage is subjected to a caustic wash.
  • Preferred materials for carrying out the caustic wash are aqueous or alcoholic sodium hydroxide and aqueous or alcoholic potassium hydroxide.
  • the caustic wash is carried out with a 30- 50% by wt. aqueous solution of the alkali, at a ratio of hydrocarbon to treating medium in the range 1:1 to 1:5 by volume.
  • the caustic wash may be carried out with a 15-25% by wt. alcoholic alkali metal hydroxide solution at a ratio of hydrocarbon to treating medium in the range 2:1 to 1:2 by volume.
  • the stage is carried out with stirring.
  • the temperature used will usually be in the range 60- C.
  • Steps which may be taken to obtain a purified microorganism or a product derived therefrom or to improve the process in respect of the production of the unmetabolised hydrocarbon fraction are described in the following applications; the use of any process step or steps therein described in association with the process herein described lies within the scope of the present invention.
  • cellular density is expressed as dry weight of yeast per litre of culture.
  • Example 1 Gram-s Diammonium phosphate 2 Potassium chloride 1.15 Magnesium sulphate, 7H O 0.65 Zine sulphate 0.17 Manganese sulphate, 1H O 0.045 Ferrous sulphate, 7H O 0.068 Yeast extract 0.025 Tap water 200 Distilled water add. 1000 ml.
  • the temperature was kept at 30i1 C., pH 4, aeration and agitation such that the aeration rate was 3 millimoles 0 per litre per hour. Addition of 10 N ammonia was by automatic pH controller.
  • Example 2 The method described in Example 1 was carried out on gas-oil from a continuous culture of Candida lipolyrim.
  • the pH was maintained at 4:01 by the automatic addition of 10 N ammonia.
  • the temperature was held at 30 C.; aeration and agitation were such that the aeration rate was 3 millimoles oxygen per litre per minute.
  • a process for the removal, at least in part, of waxes from a wax-containing petroleum gas oil which comprises, in a micro-organism growth stage, cultivating a straight chain hydrocarbon consuming-micro-organism in the presence of said wax-containing petroleum gas oil; in the presence of an aqueous nutrient medium, and in the presence of gas containing free oxygen, thereafter separating the micro-organism from the gas oil of reduced content of wax, and subjecting the gas oil to a caustic wash to reduce its cloud point.
  • yeast is of the sub-family Cryptococcoideae.

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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)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Micro-Organisms Or Cultivation Processes Thereof (AREA)
  • Gates (AREA)
US330526A 1962-12-31 1963-12-16 Process for improving cloud point of petroleum gas oil by caustic washing thereof from hydrocarbon mixtures Expired - Lifetime US3259549A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB49056/62A GB1059885A (en) 1962-12-31 1962-12-31 Process for the removal, wholly or in part, of straight chain hydrocarbons from hydrocarbon mixtures

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AT (1) AT262200B (forum.php)
BR (1) BR6355790D0 (forum.php)
DE (1) DE1545239A1 (forum.php)
FI (1) FI43860C (forum.php)
GB (1) GB1059885A (forum.php)
NO (1) NO127539B (forum.php)
SE (1) SE342834B (forum.php)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3337413A (en) * 1964-05-07 1967-08-22 Phillips Petroleum Co Solid hydrocarbon fermentation process

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US69761A (en) * 1867-10-15 Peters
US2697062A (en) * 1951-03-30 1954-12-14 Texaco Development Corp Processing of hydrocarbons
US2742398A (en) * 1951-06-09 1956-04-17 Texaco Development Corp Method of removing deposits of wax and like materials
US2868722A (en) * 1953-10-25 1959-01-13 Socony Mobil Oil Co Inc Method for producing a stabilized cracked distillate fuel oil
US2982692A (en) * 1957-06-26 1961-05-02 Hardin B Mcdill Dewaxing of oils
US2988500A (en) * 1959-03-13 1961-06-13 Universal Oil Prod Co Treatment of hydrocarbon distillates
US3069325A (en) * 1959-12-21 1962-12-18 Phillips Petroleum Co Treatment of hydrocarbons
US3152068A (en) * 1960-06-20 1964-10-06 Phillips Petroleum Co Sweetening of sour hydrocarbons

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US69761A (en) * 1867-10-15 Peters
US2697062A (en) * 1951-03-30 1954-12-14 Texaco Development Corp Processing of hydrocarbons
US2742398A (en) * 1951-06-09 1956-04-17 Texaco Development Corp Method of removing deposits of wax and like materials
US2868722A (en) * 1953-10-25 1959-01-13 Socony Mobil Oil Co Inc Method for producing a stabilized cracked distillate fuel oil
US2982692A (en) * 1957-06-26 1961-05-02 Hardin B Mcdill Dewaxing of oils
US2988500A (en) * 1959-03-13 1961-06-13 Universal Oil Prod Co Treatment of hydrocarbon distillates
US3069325A (en) * 1959-12-21 1962-12-18 Phillips Petroleum Co Treatment of hydrocarbons
US3152068A (en) * 1960-06-20 1964-10-06 Phillips Petroleum Co Sweetening of sour hydrocarbons

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3337413A (en) * 1964-05-07 1967-08-22 Phillips Petroleum Co Solid hydrocarbon fermentation process

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Publication number Publication date
FI43860B (forum.php) 1971-03-31
GB1059885A (en) 1967-02-22
NO127539B (forum.php) 1973-07-09
FI43860C (fi) 1971-07-12
SE342834B (forum.php) 1972-02-21
AT262200B (de) 1968-06-10
DE1545239A1 (de) 1969-07-31
BR6355790D0 (pt) 1973-08-28

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