Classifications

• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
  • C10M175/0025—Working-up used lubricants to recover useful products ; Cleaning by thermal processes
  • C10M175/0041—Working-up used lubricants to recover useful products ; Cleaning by thermal processes by hydrogenation processes
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
  • C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
• • 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
  • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
  • C10G2400/10—Lubricating oil

Definitions

• This invention relates to a process for re-refining used engine lubricating oils or used industrial lubricating oils containing also engine-lubricating oils.
• the expression used lubricating oil relates to engine and industrial lubricating oils which, due to their use, do not comply with their original composition.
• the known processes serving for the re-refining (regeneration) of used lubricating oils employ a regeneration process using a treatment with sulphuric-acid and bleaching earth or with a solvent or both.
• the object of these processes is to extract from the used lubricating oil the changed lubricating-oil components and the impurities, and thereby to recover in pure form the unchanged part of the primary lubricant.
• the disadvantage of these processes is that they are not economic because they work with high losses, especially if the engine-lubricating oil component of the starting material, i.e., used lubricating oil has to be recovered in a quality corresponding to that of the primary lubricant. In such cases, the losses often attain even 60%.
• the object of the invention is to eliminate the abovedescribed disadvantages and to provide a regenerating process which makes it possible to utilize the changed components, as. well as to recover in practically unchanged quantity the engine-lubricating and other lubricating components of the used lubricating oil.
• the invention resides in a process for re-refining used engine-lubricating oils or used industrial lubricating oils containing also engine-lubricating oils, comprising the steps of prepurifying the used lubricating oil with a coagulating agent and/or by vacuum distillation and subjecting' the prepurified used lubricating oil to catalytic hydrogenation under a pressure of 15 to 50, preferably 20 to 40 atm., at a temperature of 280 to 380 C., preferably 320 to 360 C., with a space velocity of 0.5 to 2.0, preferably 0.5 to 1.0 liter/liter/hour and with a gas-liquid ratio of to 120 Nm. /m. preferably 20 to 80 Nmfi/ m. in the presence of a hydrorefining catalyst and, if desired, fractionating the obtained re-refined lubricant.
• the pressure of the hydrogenation according to the invention can be varied between 20 and 40 atm., in the practice the hydrogen-rich products of the catalytic refining process can be very advantageously used under their own pressure of about 20 to 40 atm. Pure hydrogen or synthesis gas can be also advantageously employed. Used engine lubricating oils containing gas oil may also be processed according to the invention.
• a great advantage of the invention consists in the fact that, as contrasted with the conventional regeneration processes consisting of several steps, it consists but of tW steps, namely, of pre-cleaning and hydrogenation. Moreover, it ensures, at considerably lower costs, a high yield,
• Nickel oxide and molybdenum trioxide on an aluminum-oxide carrier preferably on gamma-aluminum- -oxide, can be advantageously used as catalyst.
• the catalyst may contain other metal oxides, such as ferric oxide and silica as well.
• the nickel and molybdenum oxides can be preferably used with a NiO:MoO ratio of 4l2:620.
• the following composition of the catalyst has been found very advantageous:
• NiO 4-5 parts M00 15-17 parts SiO 0-5 parts, preferably 0-2 parts 'Fe O 0-15 parts, preferably 5-10 parts.
• the process according to the invention gives a product of suitable viscosity, viscosity index, po-ur point and flash point, colour and odour.
• the oxidation stability of the product is better than that of the primary lubricants obtained by conventional methods.
• a further advantage of the invention is that it can be employed in the existing oil-hydrogenating or desulphurizing works, Without requiring new installations.
• used lubricating oils originating from mixed collection can be also employed as the basic material for the re-refining process.
• EXAMPLE 1 A used lubricating oil consisting of used engine-oils and used industrial lubricating oils and containing 7% by weight of water is treated with 5% by weight of concentrated sulphuric acid. In this Way, with a loss of 17.5% by weight, 82.5% by weight of prepurified used oil are obtained. This oil is hydrogenated at a pressure of 40 atm., a temperature of 360 C., with a space velocity of 0.5 liter/liter/hour and with a gas-liquid ratio of 0.1 Nm.
• the catalyst was heat-treated in the hydrogenation reactor in a stream of synthesis gas at 200 C., whereafter the catalyst was sulphided under a pressure of 40 atm., at a temperature of 350 C., with a space velocity of 1.0 liter/liter/hour, with a gas-liquid ratio of 0.5 Nm. /liter, with a gas oil containing 2% by weight ofbound sulphur.
• the hydrogenated product leaving the reactor is fractionated under vacuum. In this way, the following products are obtained, in percent by weight with reference to the used oil forming the starting material:
• the same used lubricating oil is prepurified by the same method and the 82.5% by weight of prepurified used oil obtained is processed by the conventional re-refining technology, that is by distilling the prepurified used oil under vacuum, extracting the fraction containing the engine oils with furfural and treating the thus-obtained solvent raflinate as well as the distillates containing lubricating oils with sulphuric acid and bleaching earth. In this way the following products are obtained:
• the thus-obtained re-refined engine oil has the following properties:
• Example 2 One proceeds as described in Example 1, with the difference that the hydrogenation is carried out at 320 C., with a space velocity of 0.5 liter/liter/hour, with a gasliquid ratio of 0.05 Nmfi/liter, under a pressure of 35 atm. with reforming gas containing 90% by volume of hydrogen and by volume of light hydrocarbons.
• the com position of the catalyst is the same as described in Example 1 but before use, the catalyst was pretreated in the hydrogenating reactor at 210 C. with synthesis gas and then it was sulphided under a pressure of atrn. at 360 C. with synthesis gas containing 2% by weight of CS In this manner the following products are obtained:
• Viscosity index Conradson residue percent by weight 0.15
• EXAMPLE 4 One proceeds as described in Example 3, with the difference that the distillation residue is hydrogenated at a temperature of 355 C., with a space velocity of 0.25 liter/ liter/ hour, with a gas-liquid ratio of 0.12 Nm. liter, under a pressure of 20 atm. with synthesis gas containing 75% by volume of hydrogen and 25% by volume of nitrogen. In this Way the following products are obtained:
• Viscosity index Conradson residue percent by weight 0.18
• EXAMPLE 5 One proceeds as described in Example 1, with the difference that the hydrogenation is carried out at 350 C. with a space velocity of 0.8 liter/liter/hour, with a gasliquid ratio of 0.1 Nmfi/ liter, under a pressure of 50 am. with synthesis gas containing 75 by volume of hydrogen and 25% by volume of nitrogen.
• the thus-obtained re-refined engine oil has the following properties:
• a process for re-refining used engine lubricating oils and used industrial lubricating oils containing such engine lubricating oils comprising the step of prepurifying the used lubricating oil by treatment with sulphuric acid; then subjecting the oil to catalytic hydrogenation at a pressure between 20 and 40 atmospheres, at a temperature between 280 and 380 C., at a space Velocity of 0.5 to 2.0 liters per liter-hour and at a gas-to-liquid ratio of 10 to 120 Nmfi/m. in the presence of a preactivated, sulphided hydro-refining catalyst.
• hydro-refining catalyst consists of 4 to 5% by weight of NiO, 15 to 17% by Weight of M00 0 to 5% by Weight of Si0 and 0 to 15% by Weight of Fe O the said catalyst being deposited on an alumina carrier and being activated, before use, at

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Combustion & Propulsion (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Organic Chemistry (AREA)
• Physics & Mathematics (AREA)
• Thermal Sciences (AREA)
• Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
• Catalysts (AREA)
• Lubricants (AREA)

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Citations (3)

• 1965
  • 1965-11-29 AT AT1073265A patent/AT268492B/de active
  • 1965-11-29 DE DE1545260A patent/DE1545260C3/de not_active Expired
  • 1965-11-30 US US510684A patent/US3346483A/en not_active Expired - Lifetime
  • 1965-11-30 GB GB50819/65A patent/GB1124260A/en not_active Expired

Patent Citations (3)

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