GB1599197A - Refining of heavy petroleum distillates - Google Patents
Refining of heavy petroleum distillates Download PDFInfo
- Publication number
- GB1599197A GB1599197A GB25479/78A GB2547978A GB1599197A GB 1599197 A GB1599197 A GB 1599197A GB 25479/78 A GB25479/78 A GB 25479/78A GB 2547978 A GB2547978 A GB 2547978A GB 1599197 A GB1599197 A GB 1599197A
- Authority
- GB
- United Kingdom
- Prior art keywords
- oil
- acid
- acid residue
- hours
- drawn
- 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
Links
- 238000007670 refining Methods 0.000 title claims description 15
- 239000003209 petroleum derivative Substances 0.000 title claims description 14
- 239000003921 oil Substances 0.000 claims description 77
- 239000002253 acid Substances 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 18
- 238000011282 treatment Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000001117 sulphuric acid Substances 0.000 claims description 12
- 235000011149 sulphuric acid Nutrition 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000080 wetting agent Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000002480 mineral oil Substances 0.000 claims description 10
- 235000010446 mineral oil Nutrition 0.000 claims description 10
- 239000000295 fuel oil Substances 0.000 claims description 9
- 239000010705 motor oil Substances 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- 241001550224 Apha Species 0.000 claims description 6
- 238000012505 colouration Methods 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 239000010802 sludge Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- 241001465754 Metazoa Species 0.000 claims description 3
- 239000010763 heavy fuel oil Substances 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 235000013311 vegetables Nutrition 0.000 claims description 3
- 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 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000007900 aqueous suspension Substances 0.000 claims description 2
- 238000004061 bleaching Methods 0.000 claims description 2
- 230000003226 decolorizating effect Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 239000011269 tar Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims 1
- 239000000194 fatty acid Substances 0.000 claims 1
- 229930195729 fatty acid Natural products 0.000 claims 1
- 150000004665 fatty acids Chemical class 0.000 claims 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002193 fatty amides Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
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
- C10G17/00—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge
- C10G17/02—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge with acids or acid-containing liquids, e.g. acid sludge
-
- 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
- C10G17/00—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge
- C10G17/02—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge with acids or acid-containing liquids, e.g. acid sludge
- C10G17/04—Liquid-liquid treatment forming two immiscible phases
- C10G17/06—Liquid-liquid treatment forming two immiscible phases using acids derived from sulfur or acid sludge thereof
Landscapes
- 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)
- Fats And Perfumes (AREA)
- Lubricants (AREA)
Description
(54) REFINING OF HEAVY PETROLEUM DISTILLATES
(71) We, ETABLISSEMENTS GEERAERT & MATTHYS RAFFINERIE KALOR, a French body corporate, of 48-50, rue des Forts, 59210 Coudekerque-Branche, France, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- The present invention is concerned with the refining of heavy petroleum distillates.
Heavy petroleum distillates are conventionally refined by treatment with sulphuric acid or oleum and removing the resulting acid residue, the treatment being generally repeated several times, fresh sulphuric acid or oleum being added each time.
The acid residues, generally referred to as acid sludges, are usually discarded, for example, in abandoned quarries or or waste land, or incinerated ih furnaces. This is likely to cause serious environmental pollution as well as waste, since the acid sludges contain a large amount of sulphuric acid and entrained oil.
We have now developed a process in which the above disadvantages are alleviated.
According to the invention, there is provided a process for refining a heavy petroleum distillate, and recovery of residues therefrom, which comprises:
(a) refining a heavy petroleum distillate by mixing the distillate with excess concentrated sulphuric acid or oleum and separating the resulting refined oil from the resulting acid residue;
(b) refining further heavy petroleum distillate or a succession of batches of heavy petroleum distillate by mixing the distillate or each batch, respectively, with the acid residue resulting from the preceding refining step (a) or (b) and separating the or each refined oil from its associated acid residue;;
(c) mixing the acid residue from the last of refining steps (b) with dehyrated spent industrial or engine oil so as to obtain a regenerated oil or with an oily residue in the presence of water and a wetting agent so as to obtain a substitute fuel oil; and
(d) optionally, when the acid residue is mixed with a dehydrated spent oil in step (c), separating the treated oil from the resulting acid residue and mixing the latter acid residue with an oily residue in the presence of water and a wetting agent so as to obtain a substitute fuel oil.
Each of mixing steps (a) to (d) is preferably carried out with vigorous stirring.
In step (a), the amount of sulphuric acid or oleum may be up to 50%, for example 3 to 50%, based on the weight of the distillate being refined. The refined oil from step (a) is preferably allowed to separate from the acid residue, neutralised (for example, with an organic or inorganic base or with a neutralising earth), decolourised and filtered so as to produce white oil of technical or medicinal quality.
Similarly, the refined oil from the or each step (b) is preferably neutralised (as in step (a)), decolourised and filtered so as to produce while oil of technical quality.
In step (c), the dehydrated spent oil has preferably been hydrated by heating to 150 to 180 C, the dehydrated oil being cooled before use in step (c). The treated spent oil from step (c) may be neutralised, decolourised and filtered (as in step (a)) to produce the regenerated oil, the latter being useful, for example, in the production of engine oils or industrial greases.
In step (c) or (d), the oily residue may be mixed with the acid residue in the presence of water and a wetting agent and the resulting mixture is heated to its boiling point with stirring, and neutralised in order to obtain a mixture of an oil phase, an aqueous phase and a neutral sludge. The substitute fuel, which may be used industrially in admixture with heavy fuel oil, is recovered by separating the resulting oil phase from the aqueous phase and the neutral sludge.
The only residue used in step (c) or (d) may be of various types, for example, it may be of mineral, vegetable, animal or synthetic origin, or a mixture thereof. A particularly preferred wetting agent for use in step (c) or (d) is a mixture of sodium arylalkyl-sulphonate, triethanolamine, fatty amides and oxy ethylated octylephenol having 9 to 15 molecules of ethylene oxide per molecule of octyl phenol. Such a wetting agent is available from us under the Trade Mark "Kalormousse 28".
It will be apparent that when the abovedescribed preferred procedure is used, the only residues for disposal can be neutral sludges, and that very little of the refined distillate is wasted.
In order that the invention may be more fully understood, the following Example, in which all percentages are by weight, is given by way of illustration only.
EXAMPLE (a) Manufacture of medicinal white oil
A vat equipped with mixing blades and valves for drawing off liquids at different levels was charged by means of a pump first with 1,000 kg of paraffin mineral oil of flash point 1 98'C, viscosity at 50"C 11 centistokes and density at 15"C 0.830 gm/cm3 and then with 500 kg of oleum at 20"C. The contents of the vat were mixed for 4 hours, after which the mixture was allowed to separate for 24 hours. After this time, 960 kg of oil were drawn off through the upper level valve (this representing a loss of 4% after acid treatment).This drawn-off oil was treated in an attached vat by neutralising by mixing for 4 hours with 40 kg of calcium carbonate (4%) in the form of a 40% aqueous suspension separating for 24 hours, drawing off the aqueous phase, decolourising the oil with 3% of super-activated bleaching earth, and filtering on a filter press.
The oil thus obtained satisfied the following Codex standards for medicinal white oils:
colouration less than 5 APHA, and
Codex acid test.
(b) Manufacture of white oil of technical grade
The acid residue from the first treatment which remained in the vat (after the oil treated in step (a) had been drawn off) and which was a sulphuric sludge composed of sulphuric acid, residual mineral oil, impurities and acid tars, was used as such for the treatment of a second batch of paraffin mineral oil of the same grade as in step (a).
For this purpose, 1000 kg of the paraffin mineral oil were again introduced into the vat and this oil and this acid residue were mixed for 4 hours; the mixture obtained was allowed to separate for 24 hours and 961 kg of oil were drawn off through the upper level valve (this representing a loss of 3.9% of oil after the acid treatment).
After the drawn-off oil has been neutralised, decolourised and filtered as described previously, a white oil of technical grade, having a colouration of5 APHA and giving a straw-yellow acid test, was obtained.
The acid residue remaining in the vat after the second treatment was again mixed for 4 hours with a third batch of 1,000 kg of mineral oil of the same grade as above: the mixture obtained was allowed to separate for 24 hours and the oil was drawn off, neutralised, decolourised and filtered as described above. 960 kg of white oil of H2 25 technical grade having a colouration of 5 APHA and giving a light brown acid test, were obtained.
(c) Manufacture of regenerated oil from spent engine oils or industrial oils
The acid residues remaining in the vat after the third treatment was mixed for 4 hours with 1,000 kg of spent engine oil which has been dehydrated by heating at 150-1 80'C and then cooled before treatment. After allowing the mixture to separate for 24 hours, 1,000 kg of treated oil were drawn off and sent into an attached vat; this oil was neutralised with calcium carbonate (0.5%) and neutralising earth (about 5%) and then decolourised with super-activated earth (about 3%) and filtered as described previously.
The oil obtained (1,000 kg) was a regenerated oil of a comparable grade to that of an engine oil obtained by direct treatment with sulphuric acid.
(d) Manufacture of a fuel oil substitute Finally, the acid residue resulting from the preceding treatments was used for the manufacture of a fuel oil substitute.
This acid residue was mixed with 10 tonnes of oil residues of various types (mineral, animal. vegetable and synthetic), 3,000 litres of water and 200 kg of the above mentioned 'iKalormousse 28" wetting agent.
The mixture was heated to its boiling point (100"C) whilst stirring, and then neutralised with ammonia to a pH of between 6 and 7.
The mixture was allowed to separate and the water which has settled out was drawn off.
The supernatant phase was then drawn off through a metal filter, having a mesh size of less than 200 microns, to give 10 tonnes of heavy fuel oil substitute having the following characteristics:
sulphur content 1.05%
viscosity at 50"C 32 cSt pH 7.9
acid number 27
water content 0.9%
The waste neutral sludges were burned in an incinerator.
WHAT WE CLAIM IS:
1. A process for refining a heavy petroleum distillate and recovery of residues therefrom, which comprises:
(a) refining a heavy petroleum distillate by mixing the distillate with excess concentrated sulphuric acid or oleum and separating the resulting refined oil from the resulting acid residue;
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (9)
1. A process for refining a heavy petroleum distillate and recovery of residues therefrom, which comprises:
(a) refining a heavy petroleum distillate by mixing the distillate with excess concentrated sulphuric acid or oleum and separating the resulting refined oil from the resulting acid residue;
(b) refining further heavy petroleum distillate or a succession of batches of heavy petroleum distillate by mixing the distillate or each batch, respectively, with the acid residue resulting from the preceding refining step (a) or (b) and separating the or each refined oil from its associated acid residue;
(c) mixing the acid residue from the last of refining steps (b) with dehydrated spent industrial or engine oil so as to obtain a regenerated oil or with an oily residue in the presence of water and a wetting agent so as to obtain a substitute fuel oil; and
(d) optionally, when the acid residue is mixed with a hydrated spent oil in step (c), separating the treated oil from the resulting acid residue and mixing the latter acid residue with an oily residue in the presence of water and a wetting agent so as to obtain a substitute fuel oil.
2. A process according to claim 1, in which the amount of sulphuric acid or oleum used in step (a) is 3 to 50%, based on the weight of the distillate.
3. A process according to claim 1 or 2, in which the refined oil from step (a) is neutralised, decolourised and filtered so as to produce white oil of technical or medicinal quality.
4. A process according to any of claims 1 to 3, in which the refined oil from the or each step (b) is neutralised, decolourised and filtered so as to produce white oil of technical quality.
5. A process according to any of claims 1 to 4. in which rhe dehydrated spent oil has been dehydrated by heating to 150 to 180 C and then cooled before use in step (c).
6. A process according to any of claims I to 5, in which, in step (c), the treated spent oil is separated from the acid residue and neutralised, decolourised and filtered so as to produce the regenerated oil.
7. A process according to any of claims 1 to 6, in which, in step (c) or (d), the acid residue is mixed with the oil residue in the presence of water and a wetting agent, the mixture is heated to its boiling point, with stirring, and neutralised, the substitute fuel oil being recovered by separating the resulting oil phase from the aqueous phase and neutral sludge.
8. A process according to any of claims I to 7. in which the wetting agent is a mixture of sodium arylalkylsulphonate, triethanolamine, fatty acids and oxyethylated octylphenol containing 9 to 15 molecules of ethylene oxide per molecule of octyl phenol.
9. A process according to claim 1, substantially as herein described in the Example.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7717083A FR2393051A1 (en) | 1977-06-03 | 1977-06-03 | PROCESS FOR TREATMENT WITH SULFURIC ACID OF HEAVY PETROLEUM DISTILLATES, USED OILS AND OTHER FATTY RESIDUES |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1599197A true GB1599197A (en) | 1981-09-30 |
Family
ID=9191667
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB25479/78A Expired GB1599197A (en) | 1977-06-03 | 1978-05-31 | Refining of heavy petroleum distillates |
Country Status (10)
| Country | Link |
|---|---|
| BE (1) | BE867774A (en) |
| DE (1) | DE2824337A1 (en) |
| DK (1) | DK247578A (en) |
| ES (1) | ES470478A1 (en) |
| FR (1) | FR2393051A1 (en) |
| GB (1) | GB1599197A (en) |
| IE (1) | IE46919B1 (en) |
| IT (1) | IT1098303B (en) |
| LU (1) | LU79752A1 (en) |
| NL (1) | NL7806063A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113046165A (en) * | 2021-03-31 | 2021-06-29 | 武汉工程大学 | Regeneration treatment method of waste lubricating oil |
-
1977
- 1977-06-03 FR FR7717083A patent/FR2393051A1/en active Granted
-
1978
- 1978-05-31 GB GB25479/78A patent/GB1599197A/en not_active Expired
- 1978-06-02 IT IT24176/78A patent/IT1098303B/en active
- 1978-06-02 LU LU79752A patent/LU79752A1/en unknown
- 1978-06-02 ES ES470478A patent/ES470478A1/en not_active Expired
- 1978-06-02 IE IE1121/78A patent/IE46919B1/en unknown
- 1978-06-02 BE BE188290A patent/BE867774A/en not_active IP Right Cessation
- 1978-06-02 DK DK247578A patent/DK247578A/en not_active Application Discontinuation
- 1978-06-02 NL NL7806063A patent/NL7806063A/en not_active Application Discontinuation
- 1978-06-02 DE DE19782824337 patent/DE2824337A1/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113046165A (en) * | 2021-03-31 | 2021-06-29 | 武汉工程大学 | Regeneration treatment method of waste lubricating oil |
Also Published As
| Publication number | Publication date |
|---|---|
| IT1098303B (en) | 1985-09-07 |
| FR2393051B1 (en) | 1982-06-11 |
| IT7824176A0 (en) | 1978-06-02 |
| IE781121L (en) | 1978-12-03 |
| DE2824337A1 (en) | 1978-12-07 |
| FR2393051A1 (en) | 1978-12-29 |
| IE46919B1 (en) | 1983-11-02 |
| BE867774A (en) | 1978-12-04 |
| DK247578A (en) | 1978-12-04 |
| LU79752A1 (en) | 1978-11-28 |
| NL7806063A (en) | 1978-12-05 |
| ES470478A1 (en) | 1979-09-01 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed [section 19, patents act 1949] | ||
| PCNP | Patent ceased through non-payment of renewal fee |