CN102443416A - Lubricating oil basic oil production method - Google Patents
Lubricating oil basic oil production method Download PDFInfo
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- CN102443416A CN102443416A CN2010105093841A CN201010509384A CN102443416A CN 102443416 A CN102443416 A CN 102443416A CN 2010105093841 A CN2010105093841 A CN 2010105093841A CN 201010509384 A CN201010509384 A CN 201010509384A CN 102443416 A CN102443416 A CN 102443416A
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Abstract
The invention discloses a lubricating oil basic oil production method. Under the condition of hydrogenation isomerism, raw material oil and hydrogen gas pass through a hydrogenation isomerism catalyst bed layer, hydrogenation isomerism catalysts comprise TON type molecular sieves and platinum group metal active ingredients, the weight content of the platinum group metal active ingredients in the hydrogenation isomerism catalysts is 0.05 weight percent to 0.5 weight percent, and the hydrogenation isomerism catalyst bed layer sequentially comprises regeneration catalysts and fresh catalysts according to the flowing direction of raw material oil and hydrogen gas. Compared with the prior art, the method has the advantages that the integral reaction performance is high, the stable operation is favorably realized, and the industrial production cost is reduced.
Description
Technical field
The invention discloses a kind of production method of lube base oil, particularly hydroisomerizing is produced the method for lubricant base.
Background technology
Contain the higher macromole straight chain of a large amount of fusing points or few branched paraffin (being called wax here) in the lubricating oil distillate, so its pour point is high, viscosity index is low and poor performance at low temperatures.Thereby, will remove high melting-point wax wherein.Process for dewaxing commonly used at present mainly contains solvent dewaxing, catalytic dewaxing and isomerization dewaxing.
Solvent dewaxing is exactly to utilize the solubility property of wax in solvent to remove, and the shortcoming of this method is that solvent is selected difficulty, a large amount of organic solvent, harmful and contaminate environment, facility investment and the process cost height of waste.Catalytic dewaxing makes wax generation catalytic cracking in the lubricating oil distillate exactly; Generation is than the hydro carbons of small molecules; Thereby make the base oil depression of pour point; P.4247388, U.S. Pat just is to use the method for catalytic dewaxing with USP.4659311, the shortcoming of this method is owing to be converted into small-molecule substance to a large amount of macromolecular cpds, makes that base oil yield is low, the viscosity index loss is big, by product value is low.Compare with preceding two kinds of process for dewaxing; Isomerization dewaxing is to make macromole wax generation isomerization reaction generate isoparaffin; And isoparaffin and the wax phase of same molecular amount pour point lower and high viscosity index than having; And still be retained in the lubricating oil distillate, thereby base oil yield is greatly enhanced, receive great concern and many documents and patent report are arranged.
At present a lot of about the report of isomerization dewaxing catalyst; For example; U.S. Pat P5990371, USP5833837, USP5817907, USP5149421, USP5135638, USP5110445, USP4919788, USP4419420, USP4601993, USP5699162, USP4518485 etc. have reported that relating to the isomerization dewaxing technology produces lubricant base; Use therein acidic components mainly contain MOR, SAPO-11, SAPO-31, SAPO-41, ZSM-22, ZSM-23, SSZ-32, Nu-10, KZ-2 and ISI-1 etc., and these materials can both make paraffinic hydrocarbon generation isomerization reaction to a certain extent.
Chinese patent CN1609175A discloses a kind of hydrotreating catalyst and preparation method thereof, and its acidic components adopt the TON structure molecular screen, and the hydrogenation metal component is one or more in Pt, Pd, Ru, Rh, nickel, cobalt, molybdenum and the tungsten.Its bullion content is up to 0.6wt%, and under certain appreciation condition, its base oil yield is 82.3%, viscosity index 105, condensation point-21 ℃.
Chinese patent CN1952073A discloses a kind of lubricating oil and has faced hydrogen dewaxing catalyst and preparation method thereof; Its acidic components have TON and MFI structural performance simultaneously, and the hydrogenation precious metal is Pd, and its content is 0.1wt%～2.0wt%; Under certain appreciation condition; Its base oil yield is 80%, viscosity index 106, condensation point-22 ℃.
Chinese patent CN1762594A discloses a kind of catalyst for hydroisomerizing paraffin and preparation method thereof, and its acidic components are ZSM-22/SAPO-11 composite molecular screen, ZSM-23/SAPO-11 composite molecular screen, EU-1/SAPO-11 composite molecular screen and NU-87/SAPO-11 composite molecular screen.The content of its precious metals pt is 0.5wt%, is raw material with the n-dodecane, and transformation efficiency is～85%, isomerizing selectivity～75%.
Isomerization dewaxing is to adopt the dual-function catalyst with special pore structure to make HMP long-chain n-praaffin and polycyclic naphthene hydrocarbon in the wax component be converted into the isoparaffin of the lower one-sided chain of fusing point and the single-ring naphthene of belt length side chain.But the alkane fusing point that isomerisation degree is high is higher on the contrary, so just must control the isomerisation degree of wax molecule.
These lubricant base production technologies adopt precious metal as hydrogenation component mostly at present, and its bullion content is higher relatively, so catalyst production cost is higher.
Summary of the invention
To the deficiency of prior art, the present invention proposes a kind of production method of lube base oil, guaranteeing the active while of reaction system, with regenerated catalyst and live catalyst grading loading, improves the combined reaction performance, reduces production costs to greatest extent.
Lube base oil producing method of the present invention comprises following content: under the hydroisomerizing condition; Raw oil and hydrogen are through the hydroisomerization catalyst bed; Hydroisomerization catalyst comprises TON type molecular sieve and platinum metals active ingredient; The weight content of platinum metals active ingredient is 0.05wt%～0.5wt% in the hydroisomerization catalyst; Be preferably 0.1wt%～0.4wt%, press raw oil and flow hydrogen gas direction, described hydroisomerization catalyst bed comprises regenerated catalyst and live catalyst successively.
In the lube base oil producing method of the present invention; Raw oil can be the various suitable raw oils in this area; Owing to use the platinum metals to be reactive metal; Generally need remove impurity such as sulphur, nitrogen in the raw oil, like the vacuum distillate of hydrocracking tail oil, hydrotreatment, the diasphaltene wet goods of hydrotreatment.
In the lube base oil producing method of the present invention, the hydroisomerizing operational condition is generally 1～15MPa for the processing condition that the technician knows like reaction pressure, and temperature of reaction is generally 280～400 ℃, and volume space velocity is generally 0.2～4h during liquid
-1, hydrogen to oil volume ratio is generally 100～1500.The concrete operations condition can require concrete definite according to feedstock property and quality product.
In the lube base oil producing method of the present invention, hydroisomerization catalyst can be selected commercial catalyst, also can be according to prior art for preparing.TON type molecular sieve in the hydroisomerization catalyst can be one or more among ZSM-22, SSZ-32, Nu-10, KZ-2 and the ISI-1 etc.; Preferably contain the ZSM-22 molecular sieve; The weight content of molecular sieve is the 10wt%～90wt% of total catalyst weight in the hydroisomerization catalyst; Preferred 30wt%～80wt%, more preferably 40wt%～70wt% can also contain inorganic refractory oxide in the hydroisomerization catalyst; Like in aluminum oxide, titanium oxide, silicon oxide, boron oxide, Natural manganese dioxide, zirconium white and the clay one or more; Inorganic refractory oxide is 5wt%～80wt% in final catalyzer content, is preferably 10wt%～60wt%, more preferably 15wt%～40wt%.The platinum family reactive metal can be in platinum, palladium, iridium, rhodium, the osmium etc. one or more, preferably contains platinum.Regeneration hydroisomerization catalyst and live catalyst can be seated in the reactor drum, also can be seated in a plurality of reactor drums.
In the inventive method, the volume ratio of regenerated catalyst and live catalyst is 1: 5～2: 1.The regenerated catalyst that regenerated catalyst obtains through regeneration for the catalyzer through hydroisomerizing reaction inactivation, the catalyzer method can be by the conventional coke-burning regeneration in this area, solvent reclamation etc., and regenerative process and condition are well known to those skilled in the art.It is active 60%～95% that the activity of regenerated catalyst is generally live catalyst, and it is active 70%～90% to be preferably live catalyst, and promptly the activation recovering rate of regenerated catalyst is 60%～95%, is preferably 70%～90%.The method of calculation of activity of such catalysts recovery rate are: during same reaction result's (is benchmark with the viscosity index); The hydrogenation reaction temperature at regenerated catalyst initial stage is consistent with live catalyst initial stage hydrogenation reaction temperature to be 100%; The hydrogenation reaction temperature at regenerated catalyst initial stage is 0 for high 60 ℃ than live catalyst initial stage hydrogenation reaction temperature, and is middle definite by linear relationship.It is active more than 95% that the activity that one skilled in the art will appreciate that regenerated catalyst generally need reach live catalyst, could reuse, and generally can't reuse for the relatively poor catalyzer of regeneration back activation recovering, can only carry out processing such as metal recovery.
The present invention adopts regenerated catalyst and live catalyst grading loading according to the characteristics of lubricant base raw material hydroisomerizing technology, has improved the W-response performance.When reaction mass contacted with catalyzer, the easy reactive component in the raw material was more, if catalyst activity is higher, was prone to take place excessive isomerization reaction and coking reaction, and is unfavorable to product property, and the steady running of catalyzer is had certain influence.After adopting regenerated catalyst and live catalyst grating, the regenerated catalyst that raw material at first contacts has suitable character, and excessive isomerization reaction does not take place easy reactive component, helps controlling side reactions such as coking yet; Along with flowing of material; During through the fresh hydroisomerization catalyst of lower floor; Be prone to RM because appropriate isomerization reaction has taken place, reactive behavior is lower than that other is difficult for iso-component in the raw material, and what therefore in highly active fresh hydroisomerization catalyst bed, take place mainly is the isomerization reaction that is difficult for iso-component in the raw material; Finally show as the W-response performance and improve, and steady running is produced favourable influence.In addition, the inventive method is because use the partial regeneration catalyzer, and the platinum metals price is very high, so the inventive method can obviously reduce the industrial production cost.
Embodiment
Be example with the hydroisomerization catalyst that contains ZSM-22 molecular sieve and reactive metal Pt below, specify the inventive method and effect.
Contain the refractory oxide aluminum oxide in the hydroisomerization catalyst, ZSM-22 molecular sieve, hydrogenation metal component Pt.Wherein the content of ZSM-22 molecular sieve is the 10wt%～90wt% of total catalyst weight, preferred 30wt%～80wt%, more preferably 40wt%～70wt%.Inorganic refractory oxide is 5wt%～80wt% in final catalyzer content, is preferably 10wt%～6wt%, more preferably 15wt%～40wt%.Active metal component is Pt, is 0.05wt%～0.5wt% in final catalyzer content, is preferably 0.1wt%～0.4wt%.
Hydroisomerization catalyst prepares according to conventional Nobel-metal catalyst preparation method.
(1) NaZSM-22 is exchanged into HZSM-22, handles the SiO of ZSM-22 molecular sieve through modifications such as dealumination complement silicons
2/ Al
2O
3Mol ratio is 80～120, specific surface area 200m
2/ g～300m
2/ g, pore volume 0.20cm
3/ g～0.40cm
3/ g, B acid amount is 0.1mmol/g～0.3mmol/g, L acid amount is 0.1mmol/g～0.2mmol/g.
(2) ZSM-22 molecular sieve, other inorganic refractory oxide, extrusion aid, peptizing agent and water are fully mixed together pinch into plastic paste, extruded moulding obtains carrier through last handling processes such as super-dry, roastings.
(3) supported active metal component on carrier through last handling processes such as drying, roastings, obtains catalyzer of the present invention.
NaZSM-22 described in the step (1) adopts ion exchange method to be exchanged into HZSM-22 earlier, and solutions employed is for containing NH
4 +Ion, NH
4 +Volumetric molar concentration is 0.05mol/L～10mol/L, and temperature is normal temperature～200 ℃, and pressure is the pressure of liquid phase for keeping solution, and the time is 1h～24h, Gu the liquid/mass ratio of solution and molecular sieve is 5～20.Dealumination process, used solution are acidic solution, wherein contain at least a be selected from mineral acid and at least a middle organic acid such as oxalic acid, acetate, Hydrocerol A that is selected from nitric acid, hydrochloric acid and the sulfuric acid etc., and mineral acid and organic acid mol ratio are 10: 1～1: 1, H in the solution
+Volumetric molar concentration is 0.05mol/L～10mol/L, and temperature is normal temperature～300 ℃, and pressure is normal pressure～5MPa, and the time is 0.5h～8h, and the mass ratio of solution and molecular sieve is 5～10.Mend the silicon process, used solution is preferably ammonium fluosilicate solution for containing the soluble silicon compound solution.Strength of solution is 1wt%～10wt%, and temperature is normal temperature～200 ℃, and pressure is normal pressure～5MPa, and the time is 0.5h～12h, and the mass ratio of solution and molecular sieve is 5～10.
Inorganic refractory oxide described in the step (2) can be selected from one or more in aluminum oxide, titanium oxide, silicon oxide, boron oxide, Natural manganese dioxide, zirconium white and the clay, is preferably aluminum oxide and/or silicon oxide, more preferably aluminum oxide.Its precursor can be selected from boehmite, pseudo-boehmite, diaspore, gipsite and visit in the aluminium stone one or more, is preferably pseudo-boehmite; Peptizing agent refers to mineral acid and/or organic acid, is preferably one or more mixtures in nitric acid, hydrochloric acid, sulfuric acid, formic acid, acetate, oxalic acid, the Hydrocerol A; Extrusion aid is meant the material that helps extrusion molding, is preferably sesbania powder, starch, CMC 99.5, carbon black, stone mill powder, Hydrocerol A etc.
The condition dry and roasting of catalyzer described in the step (3) is following: drying temperature is normal temperature～300 ℃, is preferably 100 ℃～150 ℃, and be 1～48 hour time of drying; Maturing temperature can be 400 ℃～800 ℃, is preferably 500 ℃～700 ℃, and roasting time can be 0.5～24 hour, is preferably 2～8 hours.
The inventive method is applicable to long chain alkane isomerizing and production of lube base oils.
The present invention is through using regenerated catalyst and live catalyst grading loading; With active different catalyst classification filling; Consider that the alkane that is easy to isomery in the raw material at first utilizes active low activity of such catalysts, and be difficult to the active high activity of such catalysts in alkane utilization back of isomery in the raw material, make all catalyzer in the reactor drum can both give full play to activity separately; When not reducing product property, reduce production costs to greatest extent.
Through embodiment the present invention is further specified below, it does not limit use range of the present invention, and the percentage composition that relates to is a weight percentage.
Embodiment 1
(1) processing of ZSM-22 molecular sieve
Get NaZSM-22 molecular sieve 100 gram, use 500 gram concentration be 10% ammonium nitrate solution 80 ℃ of exchanges 4 hours, repeat above-mentioned exchange then once; Use 800 gram volumetric molar concentrations to handle 4 hours at 90 ℃ as the tartaric mixing solutions of 0.2mol/L as nitric acid and the volumetric molar concentration of 0.5mol/L; Again with 1000 gram (NH
4)
2SiF
6Concentration is that 3% the aqueous solution was handled 4 hours at 85 ℃, through the HZSM-22 that filters, washing, 110 ℃ of dryings 8 hours and 550 ℃ of roastings obtained final dealumination complement silicon in 4 hours.
(2) preparation of carrier
Get above-mentioned HZSM-22 molecular sieve 650 grams, pseudo-boehmite (butt 72%) 280 grams, SB powder (butt 72%) 210 grams; Sesbania powder 20 grams mix, and add 270ml deionized water and 22ml concentrated nitric acid (66.5w%) fully mixed pinching on rolling machine then; Make it to become the paste plastic; On banded extruder, extrude the cylinder bar of diameter 1.5mm, 110 ℃ of dryings 8 hours, 550 ℃ of roastings obtained carrier in 4 hours in air atmosphere then.
(3) Preparation of Catalyst
Get the carrier that step (2) obtains, use Pt (NH
4)
4Cl
2Solution carries out saturated dipping, and then 110 ℃ of dryings 6 hours, 500 ℃ of roastings are 4 hours in air atmosphere, obtain containing the catalyzer C-1 of 0.35wt%Pt.
(4) get the hydroisomerization catalyst of same composition after the industrial application in different fortune cycles; Adopt conventional noble metal catalyst renovation process to regenerate; Be numbered ZC-1, ZC-2, ZC-3; Be respectively 78%, 85%, 92% of live catalyst through estimating its activity, do not meet the requirement of using fully separately, generally need carry out metal recovery and handle.
(5) catalyzer grading loading (volume ratio)
Catalyzer ZC-1: catalyzer C-1=1: 2.The catalyst loading situation is seen table 1,
Raw oil character is seen table 2, and appreciation condition and result see table 3.
Embodiment 2
Method for preparing catalyst is with embodiment 1, and difference is that catalyst grade prescription case is: catalyzer ZC-2: catalyzer C-1=1: 1.
Embodiment 3
Method for preparing catalyst is with embodiment 1, and difference is that catalyst grade prescription case is: catalyzer ZC-3: catalyzer C-1=2: 1.
Comparative example 1
Method for preparing catalyst is with embodiment 1, and difference is a loading catalyst C-1.
Comparative example 2
Method for preparing catalyst is with embodiment 1, and difference is a loading catalyst ZC-3.
Table 1 catalyst loading situation
| Live catalyst | Regenerated catalyst | |
| Embodiment 1 | 1 | 2 |
| Embodiment 2 | 1 | 1 |
| Embodiment 3 | 2 | 1 |
| Comparative example 1 | All | / |
| Comparative example 2 | / | All |
Table 2 raw oil character
| Project | Raw material |
| Density (20 ℃), kg/m 3 | 861.1 |
| Sulphur, μ g/g | 4.0 |
| Nitrogen, μ g/g | 1.2 |
| Viscosity (40 ℃), mm/s 2 | 29.69 |
| (100℃)，mm/s 2 | 5.47 |
| C/H | 85.82/14.08 |
| Pour point, ℃ | 21 |
| Flash-point (opening), ℃ | 198 |
| Wax content, quality % | 9.8 |
| Boiling range, ℃ (D1160) | |
| IBP/10％ | 227/399 |
| 30％/50％ | 428/441 |
| 70％/90％ | 455/469 |
| 95％/EBP | 477/500 |
Table 3 appreciation condition and result
Claims (10)
1. lube base oil producing method; Under the hydroisomerizing condition; Raw oil and hydrogen are through the hydroisomerization catalyst bed, and hydroisomerization catalyst comprises TON type molecular sieve and platinum metals active ingredient, and the weight content of platinum metals active ingredient is 0.05wt%～0.5wt% in the hydroisomerization catalyst; It is characterized in that: press raw oil and flow hydrogen gas direction, described hydroisomerization catalyst bed comprises regenerated catalyst and live catalyst successively.
2. according to the described method of claim 1, it is characterized in that: the weight content of platinum metals active ingredient is 0.1wt%～0.4wt% in the hydroisomerization catalyst.
3. according to the described method of claim 1, it is characterized in that: the hydroisomerizing reaction pressure is 1～15MPa, and temperature of reaction is 280～400 ℃, and volume space velocity is 0.2～4h during liquid
-1, hydrogen to oil volume ratio is 100～1500.
4. according to the described method of claim 1, it is characterized in that: the TON type molecular sieve in the hydroisomerization catalyst is one or more among ZSM-22, SSZ-32, Nu-10, KZ-2 and the ISI-1.
5. according to the described method of claim 1, it is characterized in that: the weight content of the TON type molecular sieve in the hydroisomerization catalyst is the 10wt%～90wt% of total catalyst weight.
6. according to the described method of claim 1, it is characterized in that: the weight content of the TON type molecular sieve in the hydroisomerization catalyst is the 30wt%～80wt% of total catalyst weight, more preferably 40wt%～70wt%.
7. according to the described method of claim 1, it is characterized in that: the volume ratio of regenerated catalyst and live catalyst is 1: 5～2: 1.
8. according to the described method of claim 1, it is characterized in that: the activity of regenerated catalyst is a live catalyst active 60%～95%.
9. according to the described method of claim 1, it is characterized in that: the activity of regenerated catalyst is a live catalyst active 70%～90%.
10. according to the described method of claim 1, it is characterized in that: raw oil is the vacuum distillate of hydrocracking tail oil, hydrotreatment or the deasphalted oil of hydrotreatment.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179490A (en) * | 2015-04-29 | 2016-12-07 | 中国石油化工股份有限公司 | A kind of renovation process of decaying catalyst |
| CN106179489A (en) * | 2015-04-29 | 2016-12-07 | 中国石油化工股份有限公司 | The renovation process of decaying catalyst |
| CN107286980A (en) * | 2016-04-05 | 2017-10-24 | 中国石油化工股份有限公司 | A kind of preparation method of lube base oil |
| CN108114666A (en) * | 2016-11-28 | 2018-06-05 | 中国石油化工股份有限公司 | The grading method of catalyst of anthraquinone hydrogenation |
| CN112090375A (en) * | 2020-08-27 | 2020-12-18 | 大唐国际化工技术研究院有限公司 | Catalytic reactor for preparing propylene from methanol and method for preparing propylene from methanol |
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| CN1952075A (en) * | 2005-10-19 | 2007-04-25 | 中国石油化工股份有限公司 | Dewaxing catalyst for lubricant oil distillate and its uses |
| CN101173193A (en) * | 2006-11-01 | 2008-05-07 | 中国石油化工股份有限公司 | Paraffinic hydrocarbon shape selecting isomerization catalyst and method for producing the same |
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| CN1609172A (en) * | 2003-10-24 | 2005-04-27 | 中国石油化工股份有限公司 | Loading method of hydroprocessing catalyst |
| CN1952075A (en) * | 2005-10-19 | 2007-04-25 | 中国石油化工股份有限公司 | Dewaxing catalyst for lubricant oil distillate and its uses |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179490A (en) * | 2015-04-29 | 2016-12-07 | 中国石油化工股份有限公司 | A kind of renovation process of decaying catalyst |
| CN106179489A (en) * | 2015-04-29 | 2016-12-07 | 中国石油化工股份有限公司 | The renovation process of decaying catalyst |
| CN106179489B (en) * | 2015-04-29 | 2018-06-15 | 中国石油化工股份有限公司 | The regeneration method of decaying catalyst |
| CN106179490B (en) * | 2015-04-29 | 2018-10-12 | 中国石油化工股份有限公司 | A kind of regeneration method of decaying catalyst |
| CN107286980A (en) * | 2016-04-05 | 2017-10-24 | 中国石油化工股份有限公司 | A kind of preparation method of lube base oil |
| CN107286980B (en) * | 2016-04-05 | 2019-03-08 | 中国石油化工股份有限公司 | A kind of preparation method of lube base oil |
| CN108114666A (en) * | 2016-11-28 | 2018-06-05 | 中国石油化工股份有限公司 | The grading method of catalyst of anthraquinone hydrogenation |
| CN112090375A (en) * | 2020-08-27 | 2020-12-18 | 大唐国际化工技术研究院有限公司 | Catalytic reactor for preparing propylene from methanol and method for preparing propylene from methanol |
| CN112090375B (en) * | 2020-08-27 | 2022-05-10 | 大唐国际化工技术研究院有限公司 | Catalytic reactor for preparing propylene from methanol and method for preparing propylene from methanol |
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