EP0816473B1 - Application d'extraits de bright stock dans les encres d'imprimerie - Google Patents

Application d'extraits de bright stock dans les encres d'imprimerie Download PDF

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Publication number
EP0816473B1
EP0816473B1 EP97116529A EP97116529A EP0816473B1 EP 0816473 B1 EP0816473 B1 EP 0816473B1 EP 97116529 A EP97116529 A EP 97116529A EP 97116529 A EP97116529 A EP 97116529A EP 0816473 B1 EP0816473 B1 EP 0816473B1
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EP
European Patent Office
Prior art keywords
bright stock
bse
carcinogenic
treat
crude
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP97116529A
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German (de)
English (en)
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EP0816473A1 (fr
Inventor
Gary Ray Blackburn
Nigel Searle
Carl Robert Mackerer
Edward Neil Ladov
Ashavir Edward Mekitarian
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ExxonMobil Oil Corp
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ExxonMobil Oil Corp
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Publication date
Application filed by ExxonMobil Oil Corp filed Critical ExxonMobil Oil Corp
Priority to DE1991633121 priority Critical patent/DE69133121T2/de
Priority to AT97116529T priority patent/ATE224941T1/de
Priority claimed from EP92903220A external-priority patent/EP0591218B1/fr
Publication of EP0816473A1 publication Critical patent/EP0816473A1/fr
Application granted granted Critical
Publication of EP0816473B1 publication Critical patent/EP0816473B1/fr
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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
    • C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
    • C10G21/003—Solvent de-asphalting

Definitions

  • the present invention relates to the use of non-carcinogenic bright stock extracts for printing ink oils and rubber extender oils.
  • Refineries do not manufacture a single lube base stock but rather process several distillate fractions and a vacuum residuum fraction. Generally, at least three distillate fractions differing in boiling range, and the residuum, may be refined. These four fractions have acquired various names in the refining art, the most volatile distillate fraction often being referred to as the "light neutral” fraction or oil. The other distillates are called “intermediate neutral” and "heavy neutral” oils.
  • the vacuum residuum, after deasphalting, solvent extraction and dewaxing, is commonly referred to as "bright stock".
  • the manufacture of lubricant base stocks involves a process for producing a slate of base stocks, which slate includes at least one refined distillate and one bright stock. Additionally, each subtractive step produces a byproduct which may be processed further or sold to an industry which has developed a use for the byproduct.
  • Crude oil is first distilled or fractionated in an atmospheric distillation tower, with residual material from the bottom of the distillation tower being further separated in a vacuum distillation tower.
  • gas and gasoline generally are recovered as overhead products of the atmospheric distillation tower, heavy naphtha, kerosene and gas oils are taken off as distillate side streams and the residual material is recovered from the bottom of the tower as reduced crude.
  • Steam may be introduced to the bottom of the tower and various side strippers used to remove light material from withdrawn heavier liquid products.
  • the residual bottom fraction or reduced crude is usually charged to a vacuum distillation tower.
  • the vacuum distillation step in lube refining provides one or more raw stocks within the boiling range of about 550°F (288°C) to 1050°F (566°C), as well as the vacuum residuum byproduct.
  • the vacuum charge is heated by a furnace means in order to vaporize a portion of the charge.
  • the preheated charge normally enters a lower portion of the vacuum tower and the vapors therefrom rise through the tower where they are cooled in selected stages producing successively lighter liquids which are separately withdrawn as the sidestream raw stock products.
  • overflash material In lube refining, excess liquid runback, known as overflash material, may be combined with the vacuum residuum and either withdrawn from the tower or charged to a deasphalting unit for further processing or dealt with in other conventional ways known to those skilled in the art.
  • the overflash material may alternatively be withdrawn, recovered and charged directly to a solvent extraction unit.
  • the presence of metallic impurities, asphaltenes and the like may render this material unsuitable far this step or likewise, for a catalytic processing step.
  • Typical vacuum distillation systems are disclosed in U.S. Patent Nos. 2 713 023, 3 886 062, 4 239 618 and 4 261 814.
  • Vacuum tower designs particularly germane to the present invention are disclosed in U.S. Patent Nos. 3 929 626 and 3 989 616.
  • each raw stock is extracted with a solvent, e.g. furfural, phenol or chlorex, which is selective for aromatic hydrocarbons, removing undesirable components.
  • a solvent e.g. furfural, phenol or chlorex
  • the vacuum residuum usually requires an additional step, typically propane deasphalting, to remove asphaltic material prior to solvent extraction.
  • the products produced for further processing into base stocks are known as raffinates.
  • the raffinate from solvent refining is thereafter dewaxed by admixing with a solvent such as a blend of methyl ethyl ketone and toluene, for example and then processed into finished base stocks.
  • the solvent extraction step separates hydrocarbon mixtures into two phases; the previously described raffinate phase which contains substances of relatively high hydrogen to carbon ratio, often called paraffinic type materials, and an extract phase which contains substances of relatively low hydrogen to carbon ratio often called aromatic type materials.
  • Solvent extraction is possible because different liquid compounds have different solution affinities for each other and some combinations are completely miscible while other combinations are almost immiscible.
  • selectivity The ability to distinguish between high carbon to hydrogen aromatic type and low carbon to hydrogen or paraffin type materials is termed selectivity. The more finely this distinguishing can be done the higher the selectivity of the solvent.
  • Furfural is typical of a suitable solvent extraction agent. Its miscibility characteristics and physical properties permit use with both highly aromatic and higher paraffinic oils of wide boiling range. Diesel fuels and light and heavy lubricating stocks are refined with furfural. Furfural exhibits good selectivity at elevated temperatures (175-250°F (79-121°C)).
  • the raw feed is introduced below or about at the center of the extraction tower. Furfural is fed into the top or upper portion of the tower. Recycled extract may be introduced into the lower section of the tower as reflux. Likewise, internal reflux is effected in the tower by the temperature gradient which is brought about by introducing the solvent at an elevated temperature and by intermediate cooling systems. Furfural solvent is recovered from the raffinate and extract phase streams or layers in suitable distillation and stripping equipment. The stripped and recovered solvent is then recycled.
  • deasphalted oils and/or aromatic extracts such as bright stock extracts which are non-carcinogenic such that contact with same will not cause the development of cancerous growths in living tissue. It would be still more desirable to produce BSE's which are free of mutagenic activity; that is, that contact with such products would not induce mutations in DNA and in living cells.
  • the invention provides a process for preparing bright stock extract which is either substantially non-carginogenic or is substantially free from mutagenic activity.
  • the invention also provides bright stock extract which is either substantially non-carcinogenic or is substantially free of mutagenic activity.
  • a non-carcinogenic bright stock extract and a non-carcinogenic deasphalted oil are provided, as well as processes for their production from reduced hydrocarbon crude feedstocks.
  • the process for the production of the non-carcinogenic bright stock extract (BSE) from a reduced hydrocarbon crude feedstock comprises establishing a functional relationship, preferably by regression, between mutagenicity index (MI) and a physical property indicative of mutagenicity for a bright stock extract stream.
  • MI mutagenicity index
  • a critical physical property level is determined which, when achieved, the resultant BSE exhibits an MI less than or equal to 1.0.
  • Process conditions are established to consistently achieve the desired BSE physical property level.
  • Reduced feedstock is then fed into a vacuum distillation column wherein the feedstock is separated into at least one product of distillation and a residuum byproduct.
  • at least a fraction of the residuum is fed into a selective solvent deasphalting unit to produce a deasphalted raffinate and an asphaltenic or tar extract.
  • At least a fraction of the deasphalted raffinate is passed through at least one solvent extraction step to reduce the deasphalted raffinate's aromatic content and to produce a bright stock raffinate and a bright stock extract, the bright stock extract having an MI less than or equal to about 1.0.
  • the BSE so produced is substantially non-carcinogenic.
  • the invention can also provide a BSE substantially free from mutagenic activity.
  • the 5% distillation boiling point has been found to be a particularly preferred physical property of the BSE for correlation with MI.
  • the critical property will be the physical property which yields a value of MI substantially equal to 1.0.
  • the critical property will be the physical property which yields a value of MI substantially equal to zero.
  • Fig. 1 is a partial lubricant refinery configuration schematically representing the steps of vacuum distillation, deasphalting and solvent extraction, wherein a blended overflash and vacuum residuum feed to a deasphalting unit is utilized.
  • Fig. 2 is a partial lubricant refinery configuration schematically representing the steps of vacuum distillation, deasphalting and solvent extraction wherein a straight vacuum residuum feed to a deasphalting unit is utilized.
  • Fig. 3 is a graph showing the relationship between Mutagenicity Index, as determined by a Modified Ames Assay, and the 5% boiling point for 19 BSE's produced in Refinery A.
  • Fig. 4 is a graph showing the relationship between Mutagenicity Index, as determined by a Modified Ames Assay, and the 5% boiling point for 5 BSE's produced by Refinery B.
  • Any lubricant refinery which utilises a solvent extraction step and/or a deasphalting step in the production of bright stocks is contemplated for use herein.
  • the process of this invention will now be described with reference to Figure 1, which schematically depicts a particularly preferred lubricant refinery partial configuration.
  • a suitable reduced crude prepared by atmospheric pressure distillation of a paraffin base or other suitable base crude oil is passed via line 1 to crude unit vacuum distillation tower 2.
  • Light ends are removed from the system via line 3.
  • a light distillate fraction, which is a raw lubricant stock, known as light neutral oil, is passed from tower 2 via line 4 either to a storage tank, not shown, or to the solvent extraction unit 22 for further processing.
  • an intermediate neutral oil is passed via line 5, and a heavy neutral oil is passed via line 6, either to storage tanks (not shown) or to solvent extraction unit 22.
  • An overflash boiling range material is withdrawn from conduit 7 located at a lower portion of the vacuum tower 2 above the reduced crude inlet conduit 1.
  • Vacuum tower residuum is withdrawn from conduit 10.
  • a portion of the vacuum tower residuum withdrawn from conduit 10 is withdrawn by conduit 12 and a portion of the overflash material withdrawn by conduit 7 is withdrawn by conduit 9.
  • These portions are withdrawn and combined in conduit 13 and passed to deasphalting unit 15, where it is treated by any of a number of useful processes, such as propane deasphalting (PDA), which is particularly preferred.
  • PDA propane deasphalting
  • the overflash material not withdrawn by conduit 9 for combining with the residuum is withdrawn by conduit 18 and may be stored in a storage tank, not shown, or solvent treated in extraction unit 22.
  • the residuum not withdrawn by conduit 12 will pass through conduit 14 and may be stored in a storage tank (not shown) or processed further as desired.
  • the deasphalted oil product, or raffinate is withdrawn through conduit 16 and, either sent for further processing into bright stock or withdrawn and stored as DAO via conduit 26.
  • the extract or tar from the deasphalting step is withdrawn through conduit 17.
  • the deasphalted oil raffinate is passed to the solvent extraction unit 22 through conduit 16 where it is treated with any one of a number of suitable solvents to remove undesirable constituents by preferential solution to produce a lubricant bright stock raffinate.
  • the bright stock raffinate so produced is passed via conduit 23 and the bright stock extract removed via conduit 24.
  • any suitable selective solvent may be used, such as furfural, phenol, chlorex, nitrobenzene, n-methyl-pyrrolidone, or others, with furfural being a particularly preferred solvent.
  • the flow from conduit 16 is halted and from either conduit 4, 5 or 6 substituted therefor.
  • the extraction unit will again remove the unwanted aromatic compounds and the light (100 SUS), intermediate (300 SUS) or heavy (700 SUS) neutral oil raffinate so produced, removed via conduit 19, 20 or 21, respectively.
  • the raffinates processed by the solvent extraction unit are dewaxed using any suitable process or stored in storage tanks (not shown) for later processing.
  • non-carcinogenic bright stock extract samples are withdrawn from conduit 24 (for the bright stock extract) during preliminary runs, or from storage tanks (not shown) where previously collected samples reside.
  • processing conditions responsible for producing a particular sample may include, but are not limited to: 1) percent of overflash material blended with crude unit vacuum tower residuum for charging the deasphalting unit; 2) the heavy-neutral distillate cut point; 3) other vacuum tower operating parameters such as steam inlet temperature, flashing zone absolute pressure and other internals; 4) deasphalting unit operating conditions, such as solvent treatment rate; 5) solvent extraction unit charge properties, such as whether blends of other streams are charged to the unit together with the deasphalted raffinate; and 6) solvent extraction unit operating conditions such as solvent treatment rate.
  • another variable worthy of note may be the crude or crude blend charged to the atmospheric distillation unit for producing the reduced crude charged to the crude unit vacuum distillation tower.
  • the bright stock extract samples collected are distilled using a standard method, such as ASTM D-1160, with preferably, at least the 5% boiling point (BP) recorded for each sample.
  • BP boiling point
  • Each sample is also tested to determine its relative mutagenicity.
  • the Modified Ames Assay procedure disclosed in U.S. Patent 4 499 187 is particularly preferred as it can rapidly and reliably determine the potential carcinogenic activity of hydrocarbon mixtures of petroleum origin.
  • Mutagenicity index data obtained from the Modified Ames tests and 5% BP data obtained from distillation tests are regressed using well-known simple linear regression techniques to develop a linear relationship between these parameters characteristic of that refinery's basic operation.
  • MI Mutagenicity index
  • Patent 4 499 187 is a ranking for relative mutagenic potential.
  • MI is the slope of the dose response curve for mutagenesis.
  • the 5% BP and MI data were linearly regressed using well-known techniques to determine the relationship between those variables. The results of this regression are shown in Figure 3. As shown in Figure 3, excellent correlation was established, with a correlation coefficient, r, of 0.92 found.
  • the 5% BP and MI data were linearly regressed to determine the relationship characteristic of Refinery B. The results of this regression are shown in Figure 4. Again, excellent correlation is achieved, with an r value of 0.88 found.
  • the critical 5% BP was found to be about 925°F (496°C) for Refinery B. Again, as at Refinery A, a BSE substantially free from mutagenic activity should be produced when the 5% BP exceeds about 978°F (526°C).
  • Refinery B's process conditions can be adjusted to achieve BSE production consistently having 5% BP's at or above the critical value of 925°F (496°C).
  • the bright stock extract can then be produced in the manner previously described.
  • non-carcinogenic BSE's can be produced.

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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)

Claims (3)

  1. Utilisation pour huile d'encre d'impression et huile diluante de caoutchouc d'un extrait d'huile de base claire qui est caractérisée par la présence de composés aromatiques, l'absence pratique de composés aromatiques polynucléaires à 3 à 7 noyaux dans leur structure et par un indice de mutagénicité inférieur à pratiquement 1,0.
  2. Utilisation selon la revendication 1, caractérisée en ce que l'indice de mutagénicité de l'extrait d'huile de base claire est sensiblement égal à 0,0, de sorte que l'extrait d'huile de base claire est sensiblement exempt d'activité mutagène.
  3. Utilisation selon la revendication 2, caractérisée en ce que l'extrait d'huile de base claire présente un point d'ébullition à 5 % supérieur à 526°C.
EP97116529A 1989-03-28 1991-06-25 Application d'extraits de bright stock dans les encres d'imprimerie Expired - Lifetime EP0816473B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE1991633121 DE69133121T2 (de) 1991-06-25 1991-06-25 Verwendung von nicht-krebserregenden Brightstock-Extrakte in Drucktinte
AT97116529T ATE224941T1 (de) 1989-03-28 1991-06-25 Verwendung von nicht-krebserregenden brightstock- extrakte in drucktinte

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP92903220A EP0591218B1 (fr) 1989-03-28 1991-06-25 Procede pour controler la preparation d'extraits de bright stock et d'huiles desasphaltees non cancerigenes

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
EP92903220A Division EP0591218B1 (fr) 1989-03-28 1991-06-25 Procede pour controler la preparation d'extraits de bright stock et d'huiles desasphaltees non cancerigenes

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EP0816473A1 EP0816473A1 (fr) 1998-01-07
EP0816473B1 true EP0816473B1 (fr) 2002-09-25

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3929626A (en) * 1974-07-31 1975-12-30 Mobil Oil Corp Production of lubricating oils blending stocks
EP0309621A1 (fr) * 1987-09-28 1989-04-05 Uop Contrôle des sous-produits aromatiques polynucléaires dans un procédé d'hydrocraquage
US4943521A (en) * 1987-02-24 1990-07-24 Mobil Oil Corporation Method for evaluating mutagenicity

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5034119A (en) * 1989-03-28 1991-07-23 Mobil Oil Corporation Non-carcinogenic bright stock extracts and deasphalted oils

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3929626A (en) * 1974-07-31 1975-12-30 Mobil Oil Corp Production of lubricating oils blending stocks
US4943521A (en) * 1987-02-24 1990-07-24 Mobil Oil Corporation Method for evaluating mutagenicity
EP0309621A1 (fr) * 1987-09-28 1989-04-05 Uop Contrôle des sous-produits aromatiques polynucléaires dans un procédé d'hydrocraquage

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Publication number Publication date
EP0816473A1 (fr) 1998-01-07

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