CN102533319A - Method for removing alkaline nitride in oil product - Google Patents
Method for removing alkaline nitride in oil product Download PDFInfo
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- CN102533319A CN102533319A CN2010106094837A CN201010609483A CN102533319A CN 102533319 A CN102533319 A CN 102533319A CN 2010106094837 A CN2010106094837 A CN 2010106094837A CN 201010609483 A CN201010609483 A CN 201010609483A CN 102533319 A CN102533319 A CN 102533319A
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- nitrogen
- oil
- auxiliary agent
- slag
- primary
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 136
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 71
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 22
- 239000002893 slag Substances 0.000 claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- 238000004062 sedimentation Methods 0.000 claims abstract description 7
- 230000000536 complexating effect Effects 0.000 claims abstract description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000008065 acid anhydrides Chemical class 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 9
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 8
- 150000002830 nitrogen compounds Chemical class 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 2
- 230000005484 gravity Effects 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 230000002787 reinforcement Effects 0.000 claims 1
- 239000003921 oil Substances 0.000 description 33
- 238000005516 engineering process Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- -1 nitrogenous compound Chemical class 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000007701 flash-distillation Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a method for removing basic nitride in oil, wherein the oil and primary nitrogen slag are fully mixed and contacted in a primary mixer to generate complex denitrification reaction, the basic nitride with strong polarity is removed, and then the oil enters a primary separation device for settlement separation, and secondary nitrogen slag is discharged to obtain primary denitrified oil and a dealkalized nitrogen auxiliary agent; after the primary denitrified oil and the dealkalized nitrogen auxiliary agent are fully mixed and react in the secondary mixer, alkaline nitrides with relatively weak polarity are removed, the alkaline nitrides enter a secondary separation device for sedimentation separation, primary nitrogen slag is discharged to obtain denitrified oil, and the primary nitrogen slag is circulated back to the primary mixer to be mixed with oil products; the primary nitrogen slag is a mixture separated after the dealkalization nitrogen auxiliary agent and the oil product are subjected to dealkalization nitrogen reaction; the dealkalized nitrogen auxiliary agent consists of the dealkalized nitrogen auxiliary agent which contains acid and acid anhydride and is described in Chinese patent CN101144031 and a complexing agent with a strengthened complexing effect; the alkali nitrogen removal rate of the oil product reaches more than 90%, and the dosage of the dealkalized nitrogen auxiliary agent can be reduced by more than 50%.
Description
Technical field
The present invention relates to a kind of method that removes oil product neutral and alkali nitride.
Background technology
The method that removes the basic nitrogen compound in the oil product has unifining and non-hydrogenation; The exploitation of unifining at present is more; And the treated oil yield is high, but this technology denitrification effect is bad, has only 10～25% with general hydrogenation catalyst nitric efficiency; Adopt extraordinary Hydrobon catalyst denitrification percent also can only reach 70～75%, and need a large amount of hydrogen sources high with expensive equipment, investment and working cost.
The main method of non-hydrogenation has: the denitrogenation of acid extraction method, solvent method denitrogenation, complexometry denitrogenation and absorption method (comprising clay-filtered) denitrogenation etc.
U.S. Pat 4960508 adopts acid, diluted acid two-step approach from oil product, to extract nitrogen heterocyclic; The concentrated acid extraction is arranged earlier; Flash distillation removes the high amounts of solvents in the concentrated acid extraction phase then; Extract with the concentrated acid extract of diluted acid after to flash distillation, diluted acid collection excess oil reclaims again, thereby has improved the selectivity of extraction and the yield of collection excess oil.
CN1088606 is a kind of liquid petroleum product solvent treatment denitrogenation method, is characterized under normal pressure, removing total nitrogen, basic nitrogen, mercaptan sulfur and low molecular organic acids in the liquid petroleum product through the liquid phase extracting.Denitrfying agent is by a kind of C
1～C
3Alcohol is formed with water or dilute alkaline aqueous solution, and total nitrogen, basic nitrogen, mercaptan sulfur decreasing ratio can reach 50～80%, and can remove the part low molecular organic acids.
US4332676 and US4332675 adopt SO
2From organic streams, remove basic nitrogen compound.Basic nitrogen compound and SO
2Form the title complex deposition with water, further precipitation separation and denitrogenation utilizes heating, inorganic solvent to handle or method SO such as inert gas purge then
2Regeneration.
CN1353167 is a kind of modified argil as denitrifying agent that is used for the refining of petroleum denitrification refining and preparation method thereof, and modified argil as denitrifying agent consists of: acidizer A5～55% (wt), complexing agent B0～30% (wt), carclazyte 20～95% (wt), water 1～15% (wt).Acidizer A and complexing agent B load on the carclazyte; Form a solid denitrfying agent; This denitrfying agent nitric efficiency is high, and the advanced nitrogen that can adopt process device identical with traditional lubrication oil white soil treating process and close processing condition to be lubricated oily base oil improves the anti-oxidative stability of lubricant base greatly; Overcome the shortcoming of liquid denitrfying agent mixing with separation difficulty, the carclazyte consumption can reduce 20-80%.
Can know that to sum up the denitrogenation of acid extraction method exists extraction selectivity low, some unazotized hydro carbons oil products also are extracted and are dissolved in the acid mutually, thereby the excess oil yield that causes coming together reduces; There is conventional solvent treatment poor selectivity in the solvent treatment denitrogenation, and when removing nitrogenous compound, a large amount of alkene also are removed, and with the raising of refining depth, the treated oil yield obviously reduces, and basic nitrogen compound removes and tends to balance; There is the little problem with frequent regeneration of adsorbents adsorb capacity in the absorption method denitrogenation.
Summary of the invention
The purpose of this invention is to provide a kind of method that removes oil product neutral and alkali nitride.
The practical implementation step is: at first oil product and a nitrogen slag are (after dealkalize nitrogen auxiliary agent and the reaction of oil product generation dealkalize nitrogen; Isolated mixture) thorough mixing contact; Remove the strong basic nitrogen compound of its Semi-polarity; Denitrogenation that the dregs of fat obtain behind separating funnel liquid-liquid separation oil and secondary nitrogen slag, denitrogenation oil again with according to improved dealkalize nitrogen auxiliary agent thorough mixing on the Chinese patent CN101144031 basis, remove polar phase to weak basic nitrogen compound; Secondary denitrogenation oil and a nitrogen slag of obtaining after the separation, one time the nitrogen slag can be recycled.Dealkalize nitrogen auxiliary agent is improved on Chinese patent CN101144031 basis, except that original acid and acid anhydrides with chain carrier, has also added and has the complexing agent of strengthening complexing action.Complexing agent comprises Fe
3+, Ni
2+, Zn
2+, Ti
2+, Cu
2+, Sn
2+In one or both.
Described mixed once device is a static mixer.
Gravity settling, electrode sedimentation or the auxiliary sedimentation means of other industry are adopted in the sedimentation of described tripping device.
Filtration unit is adopted in the separation of described tripping device, comprises whizzer, membrane filter appts or mechanical filter machine.
Adopt this technology that the basic nitrogen removal rate of oil product is reached more than 90%, and dealkalize nitrogen auxiliary dosage can reduce more than 50%.
Description of drawings
Fig. 1 removes the nitrogen slag circulation technology schema of oil product neutral and alkali nitride.
Wherein:
1 mixed once device, 2 flash liberation devices, 3 secondary mixing tanks, 4 secondary separation devices; A oil product, B secondary nitrogen slag, nitrogen slag of C, D dealkalize nitrogen auxiliary agent, E denitrogenation oil;
Embodiment
The present invention is achieved in that oil product A contacts with nitrogen slag C thorough mixing in mixed once device 1; The complexing denitrification reaction takes place, and it is settlement separate to get into flash liberation device 2 afterwards, and secondary nitrogen slag B is discharged in the bottom; A denitrogenation obtaining oil is after thorough mixing reacts secondary mixing tank 3 in dealkalize nitrogen auxiliary agent D; It is settlement separate to get into secondary separation device 4, and a nitrogen slag is discharged in the bottom, obtains basic nitrogen removal rate and reaches the denitrogenation oil E more than 90%.One time the nitrogen slag recycles.
Embodiment 1
Sulfuric acid according to 10%, 60% phosphoric acid, 20% Vanadium Pentoxide in FLAKES and 10% metals ion Cu
2+Proportioning be mixed with dealkalize nitrogen auxiliary agent, be raw material with the grand celebration coker gas oil, carry out the contrast of two kinds of dealkalize nitrogen technologies under the normal temperature and pressure conditions, test-results such as following table.
Table 1 grand celebration coker gas oil dealkalize nitrogen test-results
Annotate: grand celebration coker gas oil alkali nitrogen content 718 μ g/g.
Sulfuric acid according to 17%, 60% phosphoric acid, 15% Vanadium Pentoxide in FLAKES and 8% configuration metal ions Zn
2+Proportioning be mixed with dealkalize nitrogen auxiliary agent, be raw material with the grand celebration wax tailings, carry out the contrast of two kinds of dealkalize nitrogen technologies under 50 ℃ of temperature, the condition of normal pressure, test-results such as following table.
Table 2 grand celebration wax tailings dealkalize nitrogen test-results
Annotate: grand celebration wax tailings alkali nitrogen content 1334 μ g/g.
Hydrochloric acid according to 12%, 58% Vanadium Pentoxide in FLAKES and 30% metals ion Ti
2+Proportioning be mixed with dealkalize nitrogen auxiliary agent, be raw material with the huge port coker gas oil, carry out the contrast of two kinds of dealkalize nitrogen technologies under the normal temperature and pressure conditions, test-results such as following table.
Table 3 huge port coker gas oil dealkalize nitrogen test-results
Annotate: huge port coker gas oil alkali nitrogen content 932 μ g/g.
Oxalic acid according to 30%, 20% acetic anhydride, 30% Phenylsulfonic acid and 20% metals ion Sn
2+Proportioning be mixed with dealkalize nitrogen auxiliary agent, be raw material with Yumen coker gas oil, carry out the contrast of two kinds of dealkalize nitrogen technologies under the normal temperature and pressure conditions, test-results such as following table.
Table 4 Yumen coker gas oil dealkalize nitrogen test-results
Annotate: Yumen coker gas oil alkali nitrogen content 856 μ g/g.
Embodiment 5
Terephthalic acid according to 60%, 20% phosphorous acid and 20% metal cations Fe
2+Proportioning be mixed with dealkalize nitrogen auxiliary agent, be raw material with the huge port wax tailings, carry out the contrast of two kinds of dealkalize nitrogen technologies under 50 ℃ of temperature, the condition of normal pressure, test-results such as following table.
Table 5 huge port wax tailings dealkalize nitrogen test-results
Annotate: huge port wax tailings alkali nitrogen content 1725 μ g/g.
Claims (5)
1. method that removes oil product neutral and alkali nitride; It is characterized in that: oil product contacts with nitrogen slag thorough mixing in the mixed once device; The complexing denitrification reaction takes place, remove the strong basic nitrogen compound of its Semi-polarity, it is settlement separate to get into the flash liberation device afterwards; Discharge secondary nitrogen slag, obtain denitrogenation oil and dealkalize nitrogen auxiliary agent; Denitrogenation oil and dealkalize nitrogen auxiliary agent are in the secondary mixing tank after the thorough mixing reaction; Remove polar phase to weak basic nitrogen compound, it is settlement separate to get into the secondary separation device, discharges one time the nitrogen slag; Obtain denitrogenation oil, a nitrogen slag loops back the mixed once device to be mixed with oil product;
After one time the nitrogen slag is dealkalize nitrogen auxiliary agent and the reaction of oil product generation dealkalize nitrogen, isolated mixture;
Dealkalize nitrogen auxiliary agent is made up of with the complexing agent with reinforcement complexing action the described dealkalize nitrogen auxiliary agent that contains acid and acid anhydrides of Chinese patent CN101144031.
2. the method that removes oil product neutral and alkali nitride according to claim 1 is characterized in that: the mixed once device is a static mixer.
3. the method that removes oil product neutral and alkali nitride according to claim 1 is characterized in that: gravity settling, electrode sedimentation or the auxiliary sedimentation means of other industry are adopted in the sedimentation of tripping device.
4. the method that removes oil product neutral and alkali nitride according to claim 1 is characterized in that: filtration unit is adopted in the separation of tripping device, comprises whizzer, membrane filter appts or mechanical filter machine.
5. the method that removes oil product neutral and alkali nitride according to claim 1 is characterized in that: the complexing agent in the dealkalize nitrogen auxiliary agent is Fe
3+, Ni
2+, Zn
2+, Ti
2+, Cu
2+, Sn
2+In one or both.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010609483.7A CN102533319B (en) | 2010-12-17 | 2010-12-17 | Method for removing alkaline nitride in oil product |
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|---|---|---|---|
| CN201010609483.7A CN102533319B (en) | 2010-12-17 | 2010-12-17 | Method for removing alkaline nitride in oil product |
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| CN102533319A true CN102533319A (en) | 2012-07-04 |
| CN102533319B CN102533319B (en) | 2014-06-04 |
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|---|---|---|---|
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| Country | Link |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212489A (en) * | 2013-06-05 | 2014-12-17 | 中国石油天然气股份有限公司 | Processing method of heavy oil product with high nitrogen content |
| CN104212478A (en) * | 2013-06-05 | 2014-12-17 | 中国石油天然气股份有限公司 | Denitrification method for heavy oil product |
| CN110857392A (en) * | 2018-08-23 | 2020-03-03 | 中国石油化工股份有限公司 | Method for separating alkaline nitride from heavy oil |
| CN114471451A (en) * | 2020-10-23 | 2022-05-13 | 华东理工大学 | Preparation method and application of adsorbent for removing basic nitride from lubricating oil base oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177626A (en) * | 1997-09-10 | 1998-04-01 | 中国石油化工总公司 | Denitrification process for base oil of lubricating oil |
| CN1253165A (en) * | 1999-11-04 | 2000-05-17 | 中国石化集团武汉石油化工厂 | Refining basic oil of lubricating oil by denitrification |
| CN101121900A (en) * | 2006-08-10 | 2008-02-13 | 中国石化集团武汉石油化工厂 | Denitrogenation hydrogenation combination technique for secondary processing diesel oil |
-
2010
- 2010-12-17 CN CN201010609483.7A patent/CN102533319B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177626A (en) * | 1997-09-10 | 1998-04-01 | 中国石油化工总公司 | Denitrification process for base oil of lubricating oil |
| CN1253165A (en) * | 1999-11-04 | 2000-05-17 | 中国石化集团武汉石油化工厂 | Refining basic oil of lubricating oil by denitrification |
| CN101121900A (en) * | 2006-08-10 | 2008-02-13 | 中国石化集团武汉石油化工厂 | Denitrogenation hydrogenation combination technique for secondary processing diesel oil |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212489A (en) * | 2013-06-05 | 2014-12-17 | 中国石油天然气股份有限公司 | Processing method of heavy oil product with high nitrogen content |
| CN104212478A (en) * | 2013-06-05 | 2014-12-17 | 中国石油天然气股份有限公司 | Denitrification method for heavy oil product |
| CN104212478B (en) * | 2013-06-05 | 2016-06-08 | 中国石油天然气股份有限公司 | Denitrification method for heavy oil product |
| CN104212489B (en) * | 2013-06-05 | 2016-10-19 | 中国石油天然气股份有限公司 | Processing method of heavy oil product with high nitrogen content |
| CN110857392A (en) * | 2018-08-23 | 2020-03-03 | 中国石油化工股份有限公司 | Method for separating alkaline nitride from heavy oil |
| CN114471451A (en) * | 2020-10-23 | 2022-05-13 | 华东理工大学 | Preparation method and application of adsorbent for removing basic nitride from lubricating oil base oil |
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| CN102533319B (en) | 2014-06-04 |
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