EP0341802A1 - Abtrennung von Metallverunreinigungen aus Öl - Google Patents
Abtrennung von Metallverunreinigungen aus Öl Download PDFInfo
- Publication number
- EP0341802A1 EP0341802A1 EP89300137A EP89300137A EP0341802A1 EP 0341802 A1 EP0341802 A1 EP 0341802A1 EP 89300137 A EP89300137 A EP 89300137A EP 89300137 A EP89300137 A EP 89300137A EP 0341802 A1 EP0341802 A1 EP 0341802A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- oil
- ppm
- metal values
- aqueous solution
- solution
- 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.)
- Withdrawn
Links
- 239000002184 metal Substances 0.000 title claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 11
- 239000000356 contaminant Substances 0.000 title description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 150000001450 anions Chemical class 0.000 claims abstract description 5
- 239000008346 aqueous phase Substances 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 34
- 239000010687 lubricating oil Substances 0.000 abstract description 8
- 150000003841 chloride salts Chemical class 0.000 abstract description 3
- 150000002823 nitrates Chemical class 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000011575 calcium Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000010802 sludge Substances 0.000 description 3
- ABDKAPXRBAPSQN-UHFFFAOYSA-N veratrole Chemical compound COC1=CC=CC=C1OC ABDKAPXRBAPSQN-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 101100352919 Caenorhabditis elegans ppm-2 gene Proteins 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
Definitions
- This invention relates to the removal of metal values from oil.
- the invention relates to the removal of contaminants from vacuum residue which is the final residue oil produced by the Kellog or Synthol process.
- the invention relates to the removal of metal values that may still be present in a lubricating or other oil.
- a final residue oil is produced which is commonly referred to as vacuum residue.
- This oil generally contains a significant amount of incombustible material called ash, and this is primarily the iron catalyst used in the process, together with some inorganic salts and other incombustible materials.
- used lubricating oils contain additives and ingressed metals.
- the vacuum residue was heated to a temperature of about l00°C and then blended with water and the aqueous phase and the aqueous/ash phases were separated by centrifuge and the oil phase recovered.
- the ash content could be reduced from 2500ppm to about 600ppm which was satisfactory for certain purposes but for others required further treatment.
- an oil containing an ash content is treated with an aqueous solution of an anion capable of reacting with the metal values present to form water-soluble salts, and separating the aqueous phase from the oil phase.
- the separation is preferably carried out by centrifugation.
- the preferred an ions for use in the present invention are halides, and particularly chlorides, or nitrates.
- the oil is treated with a solution of ammonium chloride.
- a solution containing nitric acid and sodium chloride is used. In both cases the solutions may be saturated with respect to chloride ions.
- the nitric acid may be about 6 percent.
- the reaction between the anion solution and the contaminated oil is preferably conducted at an elevated temperature, preferably at or just below the boiling point of water.
- the solution may be heated to about 80°C prior to addition.
- the ratio of solution to oil is about 1:9.
- the principal metal values in vacuum residue are sodium, calcium and iron and these are easily removed according to the present invention as chlorides or nitrates.
- This oil should then have the particulate material removed from it, by heating it to 90°C, passing it through a coarse filter and subjecting it to a high gravitational separation process such as the Alfa Laval AX 213 super centrifuge, but preferably at a G-force above 15 000 G's.
- Filtration should then be carried out using a post-centrifuge 5 micron filter to remove particulate matter with a specific gravity such as that it will float in the oil.
- the feedstocks which can be used include used lubricating oil, lube oil sludge collected from lube oil circulation centrifuges, oil sludge ex tank bottoms and the residues therefrom, miscellaneous washing processes, for example, tanker cleanings and oil drum cleaning plants.
- This oil after pre-cleaning, will typically have an ash content of between 1 and 2%, where ash is defined as the residue obtained in the ASTM D482 method ash determination.
- Pre-treated oil (as above) is heated to a temperature of 90 - 95°C, preferably using a shell and tube steam-heated heat exchanger.
- the oil is held in a suitably designed tank, fitted with a circulation/agitation system.
- a 4% by volume, heated (also at a temperature of 90°C) nitric acid solution is added.
- This nitric acid solution comprises a 28% HNO3 in water (w/w).
- This aqueous acid/oil mixture is agitated for a period until complete contact between oil/contaminants and the acid solution occurs. This normally takes one to two hours.
- the temperature of the mixing vessel is maintained at 90°C by internal or external heating coils.
- a further 25% water is added at a temperature of 90C, and mixing is continued vigorously for a period ranging from five to thirty minutes.
- This mixture is fed through an adapted high speed, three phase centrifuge which separates the oil from the contaminants.
- the water is passed to an effluent treatment plant.
- a further 25% of water is added to the oil obtained from step 3.5 in a tank fitted with a circulating/agitating system, maintaining the temperature at 90°C, using internal or external heating coils.
- This mixture is fed to a high speed, three phase centrifuge. It is optional to dose the theoretical amount of caustic soda to neutralise the remaining acid component of the oil if a fully neutralised oil is required.
- a final optional step would be to pass this oil through a high speed super-centrifuge to remove the last traces of acid.
- Waste oil comprising of a mixture of fuel oil, lube oil sludge ex the lube purifier, lube oil additives and diesel oil BEFORE AFTER Water % 1,0 0,2 Ash % 1,7 0,13 Elemental Analysis of Contaminants Fe ppm 4 000 109 Ca ppm 4 000 18 Al ppm 100 0 Si ppm 1 000 20 Na ppm 2 000 34 Va ppm 5 0 S ppm 1 600 1 300
- a used lubricating oil was processed as above. The results are as follows: BEFORE AFTER Ash % 1,25 0,03 Water % 5 0,10 Fe ppm 246 4 Ni ppm 1 0 Al ppm 25 0 P ppm 443 5 Si ppm 63 10 Na ppm 134 8 Ca ppm 1 417 11 V ppm 1 0 Cr ppm 9 0 S ppm 11 483 8 521
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)
- Processing Of Solid Wastes (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ZA881823 | 1988-03-15 | ||
| ZA881823 | 1988-03-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP0341802A1 true EP0341802A1 (de) | 1989-11-15 |
Family
ID=25579199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP89300137A Withdrawn EP0341802A1 (de) | 1988-03-15 | 1989-01-09 | Abtrennung von Metallverunreinigungen aus Öl |
Country Status (1)
| Country | Link |
|---|---|
| EP (1) | EP0341802A1 (de) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE1008468A4 (fr) * | 1994-06-28 | 1996-05-07 | Univ Bruxelles | Procede d'extraction de metaux lourds des huiles usees. |
| WO1999021946A1 (de) * | 1997-10-29 | 1999-05-06 | Metallgesellschaft Aktiengesellschaft | Regenerierung saurer reaktionsschmiermittelreste |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3607731A (en) * | 1969-04-09 | 1971-09-21 | Quvoe Chemical Ind Inc | Re-refined waste crankcase oils and method |
| US4204946A (en) * | 1979-02-12 | 1980-05-27 | Turbo Resources Ltd. | Process for removing metal contaminants from used lubricating oils |
| FR2530656A1 (fr) * | 1982-07-23 | 1984-01-27 | Sader Gabriel | Procede de traitement d'huiles usees pour leur regeneration |
| DE3514970A1 (de) * | 1985-04-25 | 1986-10-30 | Dr. Baer Verfahrenstechnik GmbH, 6230 Frankfurt | Verfahren zur metallentfernung aus metallhaltigen fetten |
-
1989
- 1989-01-09 EP EP89300137A patent/EP0341802A1/de not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3607731A (en) * | 1969-04-09 | 1971-09-21 | Quvoe Chemical Ind Inc | Re-refined waste crankcase oils and method |
| US4204946A (en) * | 1979-02-12 | 1980-05-27 | Turbo Resources Ltd. | Process for removing metal contaminants from used lubricating oils |
| FR2530656A1 (fr) * | 1982-07-23 | 1984-01-27 | Sader Gabriel | Procede de traitement d'huiles usees pour leur regeneration |
| DE3514970A1 (de) * | 1985-04-25 | 1986-10-30 | Dr. Baer Verfahrenstechnik GmbH, 6230 Frankfurt | Verfahren zur metallentfernung aus metallhaltigen fetten |
Non-Patent Citations (1)
| Title |
|---|
| PATENT JOURNAL, February 1986, page 179, left-column, no. 85/5142; & ZA-A-85 5142 (FUEL FIRING SYSTEMS (PTY) LTD) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE1008468A4 (fr) * | 1994-06-28 | 1996-05-07 | Univ Bruxelles | Procede d'extraction de metaux lourds des huiles usees. |
| WO1999021946A1 (de) * | 1997-10-29 | 1999-05-06 | Metallgesellschaft Aktiengesellschaft | Regenerierung saurer reaktionsschmiermittelreste |
| US6479439B1 (en) | 1997-10-29 | 2002-11-12 | Metallgesellschaft Aktiengesellschaft | Regenerator of acid reaction lubricant residues |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH DE ES FR GB GR IT LI LU NL SE |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 19900516 |