CN103897728B - Deep hydrogenation complementary refining method for lubricating oil base oil - Google Patents
Deep hydrogenation complementary refining method for lubricating oil base oil Download PDFInfo
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- CN103897728B CN103897728B CN201210583931.XA CN201210583931A CN103897728B CN 103897728 B CN103897728 B CN 103897728B CN 201210583931 A CN201210583931 A CN 201210583931A CN 103897728 B CN103897728 B CN 103897728B
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- alumina
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- 239000002199 base oil Substances 0.000 title claims abstract description 25
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000007670 refining Methods 0.000 title claims abstract description 6
- 239000010687 lubricating oil Substances 0.000 title abstract description 10
- 230000000295 complement effect Effects 0.000 title abstract 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 36
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 18
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003921 oil Substances 0.000 claims abstract description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 4
- 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 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 3
- 239000011734 sodium Substances 0.000 claims abstract description 3
- 239000012530 fluid Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000314 lubricant Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 238000006424 Flood reaction Methods 0.000 claims description 2
- 238000004898 kneading Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- RFLFDJSIZCCYIP-UHFFFAOYSA-L palladium(2+);sulfate Chemical compound [Pd+2].[O-]S([O-])(=O)=O RFLFDJSIZCCYIP-UHFFFAOYSA-L 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 26
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 150000001336 alkenes Chemical class 0.000 abstract description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 2
- 239000011959 amorphous silica alumina Substances 0.000 abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000011156 evaluation Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 3
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000006317 isomerization reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- LKTZODAHLMBGLG-UHFFFAOYSA-N alumanylidynesilicon;$l^{2}-alumanylidenesilylidenealuminum Chemical compound [Si]#[Al].[Si]#[Al].[Al]=[Si]=[Al] LKTZODAHLMBGLG-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a method for deep hydrogenation complementary refining of lubricating oil base oil; producing the lubricating oil base oil with photo-thermal stability by using the base oil produced by a hydrogenation method or the base oil subjected to hydrogenation isodewaxing as a raw material; catalyst in wt.%: 40.0-99.9% of aluminum oxide, 0.0-60.0% of silicon oxide and 0.1-1.0% of platinum and/or palladium components; the alumina is selected from modified gamma-alumina and modified amorphous silica-alumina, the silica is selected from modified amorphous silica-alumina, the platinum is selected from one or more of chloroplatinic acid, potassium chloroplatinate, ammonium chloroplatinate and sodium chloroplatinate, and the palladium is selected from one or more of palladium chloride, palladium sulfate, ammonium chloroplatinate and potassium chloropalladate; the method is used for deep hydrogenation saturation of aromatic hydrocarbon and olefin in base oil produced by a hydrogenation method or in lubricating oil base oil subjected to hydrogenation isodewaxing, improves the oxidation stability and light stability of products, improves the color of oil products, and prevents the pour point of the products from rising.
Description
Technical field
The present invention relates to a kind of method of lubricant base deep hydrogenation post-refining.
Background technology
In recent years, along with the develop rapidly of automotive industry, constantly increase the demand of top-grade lubricating oil, its specification of quality is also more and more higher, and product hierarchy update paces are accelerated greatly, and conventional I class base oil has been difficult to the demand meeting modulation top-grade lubricating oil.China is second largest lubricating oil country of consumption in the world, and internal lube oil factory is big and small estimates at family more than 4000, and brand has more than 6000, wherein nearly 30 of foreign capitals, and lubricating oil consumption and supply are every year between 450 ~ 6,000,000 tons.Wherein Sinopec and CNPC occupy the market share of nearly 60%; With the transnational oil evaluation that shell, Mobil, BP and Castrol are representative, in occupation of the market share of about 20%, but in occupation of the share of high-end market 80%.The most refinery of current China still adopts tradition " old three covers " explained hereafter lubricant base, and cause China I class base oil overcapacity, II/III class base oil needs the present situation of import.Only have the throughput continuing increasing II/III class base oil, the requirement of China Today market development could be met.
An important channel of improving quality of lubrication oil adopts hydrogenation method to produce lubricant base exactly.Compared with traditional " old three overlap " technique, hydrogenation method technique has the significant advantages such as adaptability to raw material is strong, good product quality, therefore becomes the mainstream technology of producing APIII/III class base oil at present.Particularly hydroisomerization dewax technology, has increased substantially base oil yield and viscosity index, has at home and abroad been applied widely in high-grade base oil production equipment in recent years while the identical pour point of acquisition.But in lubricant base hydrotreatment and isomerization dewaxing reaction process, due to the service temperature of hydrogenation process higher (being generally 340 ~ 400 ° of C), although under high pressure operate, but limit by thermodynamic(al)equilibrium, aromatic hydrocarbons particularly polycyclic aromatic hydrocarbons can not by fully saturated, even generate the condensed-nuclei aromatics of a small amount of nearly 4 ~ 7 rings, the base oil normal light stability that hydrogenation method is produced is defective, the requirement of II/III class base oil to light stability and color is very high simultaneously, therefore hydrofinishing is the requisite post-processing step of HDF of lubricating oil, its main order ground is undersaturated alkene and polycyclic aromatic hydrocarbons in hydrotreated lube base oil base oil, change its chemical constitution, chemically improve the stability of base oil in essence, to improve the oxidation stability of oil product, light stability and color.
Summary of the invention
The object of this invention is to provide a kind of method of lubricant base deep hydrogenation post-refining, with the base oil that hydrotreated lube base oil hydrogenation method is produced, particularly undersaturated alkene and polycyclic aromatic hydrocarbons in lubricant base after saturated hydrogenation isomerization dewaxing, change its chemical constitution, chemically improve the stability of base oil in essence, to improve the oxidation stability of oil product, light stability and color.
Catalyzer provided by the invention, (taking catalyzer as benchmark, wt.%): aluminum oxide 40.0 ~ 99.9%, silicon oxide 0.0 ~ 60.0%, the VIIIth main group metal component 0.1 ~ 1.0%
Catalyzer provided by the invention, aluminum oxide and silicon oxide be selected from gama-alumina, modification gama-alumina, zeolite, modified zeolite, amorphous aluminum silicide or modified amorphous sial one or more.The preferred modification gama-alumina of aluminum oxide and modified amorphous sial, the preferred modified amorphous sial of silicon oxide.
Catalyzer provided by the invention, active metal component be selected from the VIIIth main group one or more, the platinum preferably in the VIIIth main group and/or palladium.Wherein platinum comes from one or more in Platinic chloride, potassium platinichloride, ammonium chloroplatinate, sodium platinichloride, preferred Platinic chloride.Wherein palladium comes from one or more in Palladous chloride, palladous sulfate, ammonium palladic chloride, potassium palladichloride, preferred Palladous chloride.
Method for preparing catalyst provided by the invention is as follows:
(1) carrier powder mixes, and adds auxiliary agent, kneading extruded moulding, 100 ~ 150 DEG C of drying 4 ~ 8h, and 400 ~ 600 DEG C of roasting 4 ~ 8h, obtain carrier.
(2) platinum and/or palladium dipping stoste is prepared respectively, platinum and/or palladium concentration 0.1 ~ 1.0wt.%.
(3) take carrier, according to impregnating metal amount weighing dipping stoste, calculate water regain according to carrier water-intake rate, adding the water yield is that water regain deducts dipping stoste water content, floods stoste and add water to be mixed into steeping fluid.
(4) adopt vacuum-impregnated method by steeping fluid evenly abundant impregnated carrier, at 100 ~ 150 DEG C of drying 4 ~ 8h, 400 ~ 600 DEG C of roasting 4 ~ 8h, obtain required catalyzer.
Catalyzer provided by the invention needs to carry out pre-treatment, pretreatment condition before use: pressure 0.1 ~ 0.5MPa, temperature 300 ~ 500 DEG C, the residence time 2 ~ 8h, hydrogen flowing quantity 50 ~ 80ml/gmin.
Catalytic reaction condition provided by the invention: reaction pressure 5.0 ~ 16.0MPa, temperature of reaction 150 ~ 280 DEG C, volume space velocity 0.5 ~ 4.0h-1, hydrogen to oil volume ratio 100 ~ 1000:1.
Catalyzer provided by the invention, hydrogenation evaluating apparatus is raw material is evaluated with hydro-treated lube base oil, catalyzer embodies good aromatic saturation performance, and product has high oxidation stability, light stability and good color.
Embodiment
Embodiment 1
By modification gamma-aluminium oxide carrier powder, auxiliary agent and water mix according to the weight ratio of 1:0.15:1, and banded extruder is extruded into the cloverleaf pattern of diameter 1.5mm, and 120 ° of dry 4h of C, 480 DEG C of roasting 4h, obtain support of the catalyst.Prepare steeping fluid according to catalyst platinum content 0.5wt.%, adopt vacuum impregnation mode will flood homogeneous immersion support of the catalyst, 120 ° of dry 4h of C, 480 DEG C of roasting 4h, obtain catalyzer.Catalyst property is in table 1.
The catalyzer of preparation is evaluated with true raw material on hydrogenation evaluating apparatus, and catalyzer needs to carry out pre-treatment, pretreatment condition before use: pressure 0.1 ~ 0.5MPa, temperature 450 ° of C, residence time 4h, hydrogen flowing quantity 65ml/gmin.Catalyst reaction condition: reaction pressure 12.0MPa, temperature of reaction 200 ° of C, volume space velocity 2.0h
-1, hydrogen to oil volume ratio 400:1.Evaluation result is in table 2.
Embodiment 2
Modification gamma-aluminium oxide carrier powder in embodiment 1 is changed to aluminum oxide and silicon oxide weight ratio is the modification gama-alumina of 1.8:1 and the powder mix of modifying amorphous sial, other are all with embodiment 1.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 3
Catalyst metal content in embodiment 2 is changed to platinum content 0.20wt.%, and palladium content 0.05wt.% prepares steeping fluid, and temperature of reaction is changed to 220 ° of C, and other are all with embodiment 2.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 4
Palladium catalyst metal content in embodiment 3 is changed to 0.10wt.% and prepares steeping fluid, other are all with embodiment 3.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 5
Palladium catalyst metal content in embodiment 3 is changed to 0.20wt.% and prepares steeping fluid, other are all with embodiment 3.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 6
Palladium catalyst metal content in embodiment 3 is changed to 0.25wt.% and prepares steeping fluid, other are all with embodiment 3.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 7
Catalyst platinum metal content in embodiment 3 is changed to 0.30wt.% and prepares steeping fluid, other are all with embodiment 3.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 8
Palladium catalyst metal content in embodiment 7 is changed to 0.10wt.% and prepares steeping fluid, other are all with embodiment 7.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 9
Palladium catalyst metal content in embodiment 7 is changed to 0.20wt.% and prepares steeping fluid, other are all with embodiment 7.Catalyst property is in table 1, and evaluation result is in table 2.
Embodiment 10
Palladium catalyst metal content in embodiment 7 is changed to 0.25wt.% and prepares steeping fluid, other are all with embodiment 7.Catalyst property is in table 1, and evaluation result is in table 2.
Table 1 catalyst property
| Project | Than table m 2/g | Pore volume ml/g | Aperture nm |
| Embodiment 1 | 255.96 | 0.40 | 5.73 |
| Embodiment 2 | 321.12 | 0.68 | 8.57 |
| Embodiment 3 | 327.51 | 0.69 | 8.42 |
| Embodiment 4 | 323.42 | 0.69 | 8.51 |
| Embodiment 5 | 322.70 | 0.66 | 8.58 |
| Embodiment 6 | 318.76 | 0.68 | 8.57 |
| Embodiment 7 | 322.57 | 0.67 | 8.47 |
| Embodiment 8 | 321.07 | 0.68 | 8.52 |
| Embodiment 9 | 320.82 | 0.69 | 8.38 |
| Embodiment 10 | 325.65 | 0.68 | 8.49 |
Table 2 evaluating catalyst result
Claims (1)
1. a method for lubricant base deep hydrogenation post-refining, is characterized in that: the base oil produced with hydrogenation method, or with base oil after hydroisomerization dewax for raw material, produces the lubricant base of photo and thermal stability; Reaction pressure 5.0 ~ 16.0MPa, temperature of reaction 150 ~ 280 DEG C, volume space velocity 0.5 ~ 4.0h
-1, hydrogen to oil volume ratio 100 ~ 1000:1;
Catalyzer is by wt.%: aluminum oxide 40.0 ~ 99.9%, silicon oxide 0.0 ~ 60.0%, platinum and/or palladium component 0.1 ~ 1.0%, and the per-cent sum of each component is 100%;
The preparation method of catalyzer is as follows:
(1) carrier powder mixes, and adds auxiliary agent, kneading extruded moulding, 100 ~ 150 DEG C, and dry 4 ~ 8h, at 400 ~ 600 DEG C of roasting 4 ~ 8h, obtains carrier;
(2) the dipping stoste of platinum and/or palladium is prepared respectively, platinum and/or palladium concentration 0.1 ~ 1.0wt.%;
(3) take carrier, according to impregnating metal amount weighing dipping stoste, calculate water regain according to carrier water-intake rate, adding the water yield is that water regain deducts dipping stoste water content, floods stoste and add water to be mixed into steeping fluid;
(4) adopt vacuum-impregnated mode that steeping fluid is evenly fully infiltrated carrier, at 100 ~ 150 DEG C of drying 4 ~ 8h, 400 ~ 600 DEG C of roasting 4 ~ 8h, obtain catalyzer;
Need before using to carry out pre-treatment, pretreatment condition: pressure 0.1 ~ 0.5MPa, temperature 300 ~ 500 DEG C, the residence time 2 ~ 8h, hydrogen flowing quantity 50 ~ 80ml/gmin;
Described aluminum oxide is selected from modification gama-alumina and modified amorphous sial, and silicon oxide is selected from modified amorphous sial;
Described platinum come from Platinic chloride, potassium platinichloride, ammonium chloroplatinate, sodium platinichloride one or more;
Described palladium come from Palladous chloride, palladous sulfate, ammonium palladic chloride, potassium palladichloride one or more.
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| CN105420604A (en) * | 2015-11-05 | 2016-03-23 | 安徽银球轴承有限公司 | Self-lubrication sintered metal powder bearing with high tenacity and preparation method of self-lubrication sintered metal powder bearing |
| CN109395731B (en) * | 2017-08-18 | 2021-09-03 | 中国石油化工股份有限公司 | Polycyclic aromatic hydrocarbon selective hydrogenation catalyst |
| KR102009364B1 (en) * | 2018-11-02 | 2019-08-09 | 에스케이이노베이션 주식회사 | Catalyst for Hydrofinishing and Production Method of Lubricating Base Oil using Thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676585A (en) * | 2004-03-31 | 2005-10-05 | 中国石油化工股份有限公司 | Method for preparing lubricating oil base oil |
| CN101214455A (en) * | 2007-12-27 | 2008-07-09 | 长沙矿冶研究院 | Preparation method of supported nano hydrogenation catalyst |
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| US6699385B2 (en) * | 2001-10-17 | 2004-03-02 | Chevron U.S.A. Inc. | Process for converting waxy feeds into low haze heavy base oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676585A (en) * | 2004-03-31 | 2005-10-05 | 中国石油化工股份有限公司 | Method for preparing lubricating oil base oil |
| CN101214455A (en) * | 2007-12-27 | 2008-07-09 | 长沙矿冶研究院 | Preparation method of supported nano hydrogenation catalyst |
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