WO2003044141A2 - Process for the purification of contaminated oils - Google Patents

Process for the purification of contaminated oils Download PDF

Info

Publication number
WO2003044141A2
WO2003044141A2 PCT/HU2002/000119 HU0200119W WO03044141A2 WO 2003044141 A2 WO2003044141 A2 WO 2003044141A2 HU 0200119 W HU0200119 W HU 0200119W WO 03044141 A2 WO03044141 A2 WO 03044141A2
Authority
WO
WIPO (PCT)
Prior art keywords
oils
purification
adsorbent
contaminated
distillation
Prior art date
Application number
PCT/HU2002/000119
Other languages
French (fr)
Other versions
WO2003044141A3 (en
Inventor
József KOSZTA
József PASINSZKI
Tamás DÁVID
Original Assignee
Koszta Jozsef
Pasinszki Jozsef
David Tamas
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Koszta Jozsef, Pasinszki Jozsef, David Tamas filed Critical Koszta Jozsef
Priority to AU2002366004A priority Critical patent/AU2002366004A1/en
Publication of WO2003044141A2 publication Critical patent/WO2003044141A2/en
Publication of WO2003044141A3 publication Critical patent/WO2003044141A3/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning

Definitions

  • the subject of the invention is a process for the purification of contaminated oils, such as, hydrocarbon oils or polyether oils.
  • U.S. Patent 5,527,449 comprises the distillation of the mixture of waste oils, animal fats and plant oils simultaneously cracking of them.
  • the resulted unstabilized material obtained this way can not be considered as a product and according to the description it needs further processing.
  • Our target was to develop a procedure with low quantity of waste for cleaning the contaminated hydrocarbon oils and polyether oils with which the oils are purified from the toxic components and become applicable for energy-supply in ' general-purpose furnaces or become utilizable in other types of technologies.
  • Impurity components of them comprise additives (containing zinc, magnesium, calcium, aluminium, sulphur, chlorine), abrasion residues (cadmium, iron, stannum, nickel, molybdenum, chromium, lead, copper, cobalt) and degradation products formed in use.
  • the invention is based upon the recognition that after an treatment of the oils with a base, the separation of the liquid phases is not necessary, since the decomposition products in the aqueous phase can be adsorbed on an appropriate adsorbent and water can be separated by means of distillation without redissolving the impurities into the oily phase.
  • Preferred adsorbents are diatomaceous earth or zeolite. The adsorbents with adsorbed impurity components and abrasion residues can then be filtered out as mechanical impurities.
  • ammonium-hydroxide as a base makes more simple the process. Namely ammonium-hydroxide can be distilled off and recycled at the end of the process. Consequently the raw material cost of the process is lower and less dangerous waste is formed.
  • the reactor is evacuated by the compressor 3 and filled with N . Under continuous and intensive stirring the reactor is heated up to 110 °C, while the steam generated as a result of heating is transferred under 4 bar pressure by the compressor 3 through the cooler and condensed (in the reactor the operational pressure is about 0,5 bar). The condensate (water and light hydrocarbon) is collected in the drain tank 4 till the end of dripping.
  • Step 2 Degradation of impurities: Oil is then heated preferably to 150°C and from the alkali storage vessel 7 concentrated ammonia solution in a portion (w/w) from 5 to 15, preferably 10 is added to it and stirred vigorously for 30 min.
  • Step 3) Removal of ammonia solution When the heating is completed the exhaust gases of the reactor 2 are transferred by the compressor 3 through the heat exchanger 8 and condensed. In order to avoid foaming of the content of the reactor a foam sensor is installed. NH OH is condensed in the heat exchanger and till the end of dripping it is collected in the drain tank 4 and then transferred into the alkali storage vessel 7.
  • the holding tank 9 vents through the adsorbent 16.
  • Oil is transferred into the mud filter 10, where in order to build up the necessary filter cake it is circulated for 10 to 120 min, preferably for 60 min.
  • the filter cake having been built up the re-circulating section of the filtration loop is closed and from the filter the oil as a product is harvested through the heat exchanger 1 simultaneously pre-heating the sequential batch.
  • Benefit of the process of the invention is that it can be carried out very easily and small quantity of waste is obtained while the concentration of abrasion residues, zinc and aluminium compounds and halogenated aliphatic hydrocarbons of contaminated oils is reduced.

Landscapes

  • 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)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)

Abstract

The present invention relates to a process for the purification of contaminated oils, mainly hydrocarbon oils or polyether oils wherein the contaminated oil is treated by an base solution in the presence of an adsorbent and then water is removed by distillation without the separation of the liquid-phases and the impurities adsorbed on adsorbent are separated preferably by filtration. The oils purified by the process become applicable for energy-supply in commercial furnaces or become utilizable in other types of technologies.

Description

Process for the purification of contaminated oils
Field if the invention:
The subject of the invention is a process for the purification of contaminated oils, such as, hydrocarbon oils or polyether oils.
The handling of used lubricating oils (dead oils) continuously raises serious difficulties to the consumers, therefore great efforts have already been made for the purification of these wastes and for recycling them.
Background of the invention:
Extended experiments were performed in the 1970's for the regeneration of waste lubricating oils (dead oils) in Hungary, however those did not fulfil the expectations. Essentially the procedure consisted of the refinement of dead oils by sulphuric acid and then the re-admixture of them The quality of the obtained oil was very low and the regeneration procedure resulted in large quantity of wastes being dangerous to the environment, furthermore their handling and storage could hardly be solved. Further disadvantage of the procedure was that it was applicable only in cases of natural based lubricating oils having a low admixture level. Nowadays the powerful lubricating oils with high admixture levels are used and they very often made of synthetic base oils.
There are known procedures for the regeneration of the lubricating oil wastes comprising of concentrated base treatment. For example the French Patent No. 93 03275 and the Italian Patent No. MI92A002271 comprise the combination of an alkaline extraction with a batch distillation. Products of the process are the oily distillates taken at different boiling point range. Major disadvantage of the described procedures is that due to the inconsistent quality of the gathered lubricating oil wastes the manufacturing of lubrication oil in standard quality is very difficult. A further disadvantage of the processes is that the distillation residue as a waste is significantly high occasionally exceeding 30%. U.S. Patent No. 08/925 279 and German Patent No. 198 52 007 describe procedures comprising the distillation of dead oils, then the extraction of distillate. Disadvantage of the procedures are similar to the ones described previously.
The process of U.S. Patent 5,527,449 comprises the distillation of the mixture of waste oils, animal fats and plant oils simultaneously cracking of them. The resulted unstabilized material obtained this way can not be considered as a product and according to the description it needs further processing.
The process disclosed in International Patent Application No. WO 9921945 comprises the distillation of oily wastes and cracking of them under hydrogen gas introduction. In this case the product is also equal to the distillate. In this case, due to the cracking, the quantity of the distillation residue is low relative to the simple distillation procedures described above. The high price of the hydrogen gas manufactured by the decomposition of hydrocarbons considerably reduces the economy of the process.
An other problem is that since these procedures have to be carried out in large scale in refinery plants, a centralised gathering of wastes is needed for processing, which further raises the costs of the procedure.
Summary of the invention:
Our target was to develop a procedure with low quantity of waste for cleaning the contaminated hydrocarbon oils and polyether oils with which the oils are purified from the toxic components and become applicable for energy-supply in 'general-purpose furnaces or become utilizable in other types of technologies.
The oily wastes evolve mainly as a result of running down of lubricating oils. Impurity components of them comprise additives (containing zinc, magnesium, calcium, aluminium, sulphur, chlorine), abrasion residues (cadmium, iron, stannum, nickel, molybdenum, chromium, lead, copper, cobalt) and degradation products formed in use.
It is known that after the treatment of oils with concentrated base the compounds containing zinc and aluminium, furthermore halogenated aliphatic hydrocarbons degrade under the effect of bases and the decomposition products become extractable into the aqueous phase.
The invention is based upon the recognition that after an treatment of the oils with a base, the separation of the liquid phases is not necessary, since the decomposition products in the aqueous phase can be adsorbed on an appropriate adsorbent and water can be separated by means of distillation without redissolving the impurities into the oily phase. Preferred adsorbents are diatomaceous earth or zeolite. The adsorbents with adsorbed impurity components and abrasion residues can then be filtered out as mechanical impurities.
Our further recognition is that the application of ammonium-hydroxide as a base makes more simple the process. Namely ammonium-hydroxide can be distilled off and recycled at the end of the process. Consequently the raw material cost of the process is lower and less dangerous waste is formed.
A detailed demonstration of our invention is presented in the following example without limiting our claims only on it.
Example:
Step 1) Flashing point adjustment: Pre-heated 100 portion (w/w) of dead oil is introduced through the heat exchanger 2 into the reaction tank being equipped with a mixer 1. During introduction zeolite activated properly is mixed in 0.1-4 portion (w/w), preferably in 1 portion (w/w) into the oil stream. The reactor is evacuated by the compressor 3 and filled with N . Under continuous and intensive stirring the reactor is heated up to 110 °C, while the steam generated as a result of heating is transferred under 4 bar pressure by the compressor 3 through the cooler and condensed (in the reactor the operational pressure is about 0,5 bar). The condensate (water and light hydrocarbon) is collected in the drain tank 4 till the end of dripping. Phases of the collected condensate are separated and the upper phase is transferred into the hydrocarbon storage vessel 5 while the lower phase is transferred into the water storage tank 6. Condensates are handled as dangerous wastes (expected quantity is about 0-2 portion /w/w/ per batch). Explosion of the reactor is protected by the release valve 11 connected after the safety vessel 12, while other part of the equipment is protected by the release valve 13 venting through the scrubber 14 and adsorbent 15 being connected in series. Step 2) Degradation of impurities: Oil is then heated preferably to 150°C and from the alkali storage vessel 7 concentrated ammonia solution in a portion (w/w) from 5 to 15, preferably 10 is added to it and stirred vigorously for 30 min.
Step 3) Removal of ammonia solution: When the heating is completed the exhaust gases of the reactor 2 are transferred by the compressor 3 through the heat exchanger 8 and condensed. In order to avoid foaming of the content of the reactor a foam sensor is installed. NH OH is condensed in the heat exchanger and till the end of dripping it is collected in the drain tank 4 and then transferred into the alkali storage vessel 7.
Step 4) Removal of impurities: Treated oil is pumped into the holding tank 9. The holding tank 9 vents through the adsorbent 16. Oil is transferred into the mud filter 10, where in order to build up the necessary filter cake it is circulated for 10 to 120 min, preferably for 60 min. When the filter cake having been built up the re-circulating section of the filtration loop is closed and from the filter the oil as a product is harvested through the heat exchanger 1 simultaneously pre-heating the sequential batch.
Benefit of the process of the invention is that it can be carried out very easily and small quantity of waste is obtained while the concentration of abrasion residues, zinc and aluminium compounds and halogenated aliphatic hydrocarbons of contaminated oils is reduced.

Claims

Claims are:
1.) A process for the purification of contaminated hydrocarbon oils or polyether oils wherein the purification comprises the treatment by alkaline solution, preferably by ammonium- hydroxide and adding of adsorbent for yield increasing and then removal of water by distillation and the impurities by filtration.
2.) A process of claim 1 wherein the adsorbent is zeolite or diatomaceous earth.
PCT/HU2002/000119 2001-11-20 2002-11-13 Process for the purification of contaminated oils WO2003044141A2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2002366004A AU2002366004A1 (en) 2001-11-20 2002-11-13 Process for the purification of contaminated oils

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
HU0105022A HU225697B1 (en) 2001-11-20 2001-11-20 Method for purifying of used oils
HUP0105022 2001-11-20

Publications (2)

Publication Number Publication Date
WO2003044141A2 true WO2003044141A2 (en) 2003-05-30
WO2003044141A3 WO2003044141A3 (en) 2003-07-17

Family

ID=89979917

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/HU2002/000119 WO2003044141A2 (en) 2001-11-20 2002-11-13 Process for the purification of contaminated oils

Country Status (3)

Country Link
AU (1) AU2002366004A1 (en)
HU (1) HU225697B1 (en)
WO (1) WO2003044141A2 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008032129A1 (en) * 2006-09-14 2008-03-20 David Tamas Improved method for purifying contaminated oils
NO20064993L (en) * 2006-10-31 2008-05-02 Due Miljoe As Procedure for purifying oils and their use in food and feed
CN103146423A (en) * 2013-04-01 2013-06-12 佛山市和挚承环保科技有限公司 Method for regenerating and extracting waste mineral oil by filling nitrogen extracting
CN109957448A (en) * 2017-12-26 2019-07-02 丰益(上海)生物技术研发中心有限公司 A kind of crude oil cleaning technology

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1919655A (en) * 1929-07-12 1933-07-25 Bocjl Corp Purification of oil
DE2704469A1 (en) * 1977-02-03 1978-08-10 Krupp Ag Huettenwerke Reclamation of used phosphate hydraulic fluid - by treating with water, alkali and bleaching earth
WO1987004455A1 (en) * 1986-01-27 1987-07-30 Strahorn David A Process for purifying used lubricating oil
FR2703067A1 (en) * 1993-03-22 1994-09-30 Sotulub Method and installation for regenerating lubricating oils

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2619264B2 (en) * 1988-06-23 1997-06-11 トヨタ自動車株式会社 Reprocessing of lubricating waste oil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1919655A (en) * 1929-07-12 1933-07-25 Bocjl Corp Purification of oil
DE2704469A1 (en) * 1977-02-03 1978-08-10 Krupp Ag Huettenwerke Reclamation of used phosphate hydraulic fluid - by treating with water, alkali and bleaching earth
WO1987004455A1 (en) * 1986-01-27 1987-07-30 Strahorn David A Process for purifying used lubricating oil
FR2703067A1 (en) * 1993-03-22 1994-09-30 Sotulub Method and installation for regenerating lubricating oils

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 014, no. 131 (C-0700), 13 March 1990 (1990-03-13) & JP 02 004898 A (TOYOTA MOTOR CORP;OTHERS: 01), 9 January 1990 (1990-01-09) *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008032129A1 (en) * 2006-09-14 2008-03-20 David Tamas Improved method for purifying contaminated oils
NO20064993L (en) * 2006-10-31 2008-05-02 Due Miljoe As Procedure for purifying oils and their use in food and feed
CN103146423A (en) * 2013-04-01 2013-06-12 佛山市和挚承环保科技有限公司 Method for regenerating and extracting waste mineral oil by filling nitrogen extracting
CN109957448A (en) * 2017-12-26 2019-07-02 丰益(上海)生物技术研发中心有限公司 A kind of crude oil cleaning technology

Also Published As

Publication number Publication date
WO2003044141A3 (en) 2003-07-17
HUP0105022A3 (en) 2005-04-28
HU225697B1 (en) 2007-06-28
HUP0105022A2 (en) 2004-04-28
HU0105022D0 (en) 2002-01-28
AU2002366004A1 (en) 2003-06-10

Similar Documents

Publication Publication Date Title
KR101897454B1 (en) A process for separation and purification of sodium sulfide
US5045179A (en) Process for the hydrogenation reprocessing of used oils
KR20060046629A (en) Process for the working-up of waste waters containing aromatic nitro compounds
EA002638B1 (en) Method of re-refining waste oil by distillation and extraction
AU611620B2 (en) Process for extracting and disposing of nitrophenolic by-products
JP4489956B2 (en) Treatment method of halogen-containing organic waste materials
RU2356939C2 (en) Method for regeneration of spent oils by means of demetallisation and distillation
ES2383436T3 (en) Method of removal of contaminants from petroleum distillates
EP2612715B1 (en) Recovery of sulfur from sulfur-containing waste
WO2003044141A2 (en) Process for the purification of contaminated oils
EP0603400A1 (en) Method of removing halogenated aromatic compound from hydrocarbon oil
JP6498270B2 (en) Purification of used oil
US4159992A (en) Removal of plastic polymer fines from tallow
EP2024038A1 (en) Process for the regeneration of a used oil
CN102786176B (en) Comprehensive utilization method of catalytic cracking gasoline sludge
CA2185393A1 (en) Process for eliminating adsorbable organic halogen compounds from wastewaters
JPH04120197A (en) Purifying device of waste oil
WO2008032129A1 (en) Improved method for purifying contaminated oils
SU715448A1 (en) Method of sulfure extraction
KR950002824B1 (en) Fraction removing method by organic solute in sodium hydroxide solution
WO2024175435A1 (en) Process for removing contaminants from waste plastics oil
JP4065714B2 (en) Method for purifying 1,2-dichloroethane
WO2022235260A1 (en) Contaminant removal from coal tar-derived crude phenols
JPH07188672A (en) Method for refinement of tar acid
WO1995032152A1 (en) Method for purifying impure aluminium oxide by extraction

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A2

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NO NZ OM PH PL PT RO RU SD SE SG SI SK SL TJ TM TN TR TT TZ UA UG US UZ VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A2

Designated state(s): GH GM KE LS MW MZ SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LU MC NL PT SE SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
32PN Ep: public notification in the ep bulletin as address of the adressee cannot be established

Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 69(1) EPC - EPO FORM 1205A OF 26.08.04

122 Ep: pct application non-entry in european phase
NENP Non-entry into the national phase

Ref country code: JP

WWW Wipo information: withdrawn in national office

Country of ref document: JP