CN101942322B - Lubricating oil base oil producing method - Google Patents
Lubricating oil base oil producing method Download PDFInfo
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Abstract
The invention discloses a lubricating oil base oil producing method. The raw oil and the hydrogen pass through a hydroisomerization catalyst bed under the hydroisomerization condition; the hydroisomerization catalyst comprises a TON-type molecular sieve and a platinum metal active component; the weight content of the platinum metal active component in the hydroisomerization catalyst is 0.05wt%-0.5wt%; the hydroisomerization catalyst bed at least comprises two types of hydroisomerization catalysts; and the active metal content in the hydroisomerization catalyst is increased in sequence according to the flow direction of the raw oil and the hydrogen. In the invention, the catalysts with different activities are filled in grading by using different grades to fill the catalyst of the heavy metal content, thus leading the catalysts in a reactor to give fully play to respective activity, lowering the heavy metal content to a large extent while not lowering the product property, thereby lowering the production cost.
Description
Technical field
The invention discloses a kind of production method of lubricant base, particularly hydroisomerizing is produced the method for lubricant base.
Background technology
Contain macromole straight chain or few branched paraffin (referred to herein as wax) that a large amount of fusing points is higher in 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 mainly contains solvent dewaxing, catalytic dewaxing and isomerization dewaxing at present.
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, wasted a large amount of organic solvents, harmful and contaminate environment, facility investment and process cost are high.Catalytic dewaxing makes wax generation catalytic cracking in lubricating oil distillate exactly, generate more micromolecular hydro carbons, thereby make the base oil depression of pour point, P.4247388, U.S. Pat is exactly the method for using catalytic dewaxing with USP.4659311, the shortcoming of this method is because the macromolecular cpd a large amount of is converted into small-molecule substance, makes that base oil yield is low, the viscosity index loss is large, by product is worth low.With the first two process for dewaxing, compare, isomerization dewaxing is to make macromole wax generation isomerization reaction generate isoparaffin, and isoparaffin and the wax phase of the same molecular amount pour point lower than having and high viscosity index, and still be retained in lubricating oil distillate, thereby base oil yield is greatly enhanced, is paid close attention to greatly and many documents and patent report 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 Isodewaxing 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., 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 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, the hydrogenation precious metal is Pd, 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%, take n-dodecane as raw material, and transformation efficiency is～85%, isomerization selectivity～75%.
Isomerization dewaxing is the isoparaffin that adopts the dual-function catalyst with special pore structure to make high-melting-point long-chain n-praaffin in the wax component and polycyclic naphthene hydrocarbon be converted into the one-sided chain that fusing point is lower 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 Production Technology of Lubricating Base Oils adopt precious metal as hydrogenation component mostly at present, and its bullion content is relatively high, so the production cost of catalyzer is higher.
Summary of the invention
For the deficiencies in the prior art, the present invention proposes a kind of production method of lubricant base, when guaranteeing the reaction system activity, adjusts catalyzer and forms, and improves the combined reaction performance, reduces to greatest extent bullion content, reduces production costs.
Lubricating oil base oil producing method of the present invention comprises following content: under the hydroisomerizing condition, stock oil and hydrogen are by the hydroisomerization catalyst bed, hydroisomerization catalyst comprises TON type molecular sieve and platinum metals active ingredient, in hydroisomerization catalyst, the weight content of platinum metals active ingredient is 0.05wt%～0.5wt%, be preferably 0.1wt%～0.4wt%, described hydroisomerization catalyst bed at least comprises two kinds of hydroisomerization catalysts, press stock oil and flow hydrogen gas direction, in hydroisomerization catalyst, active metallic content increases successively.In the hydroisomerization catalyst that metal content increases successively, in adjacent hydroisomerization catalyst, the weight content of hydrogenation active metals differs 0.02wt%～0.2wt%.
In Lubricating oil base oil producing method of the present invention, stock oil can be the various suitable stock oil in this area, owing to using platinum metals, it is reactive metal, generally need remove the impurity such as sulphur, nitrogen in stock oil, as the vacuum distillate of hydrocracking tail oil, hydrotreatment, the diasphaltene wet goods of hydrotreatment.
In Lubricating oil base oil producing method of the present invention, the hydroisomerizing operational condition is processing condition known by the technical staff, and as reaction pressure is generally 1～15MPa, temperature of reaction is generally 280～400 ℃, and during liquid, volume space velocity is generally 0.2～4h
-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 Lubricating oil base oil producing method of the present invention, hydroisomerization catalyst can be selected commercial catalyst, also can prepare according to prior art.TON type molecular sieve in hydroisomerization catalyst can be ZSM-22, SSZ-32, Nu-10, one or more in KZ-2 and ISI-1 etc., preferably contain the ZSM-22 molecular sieve, 10wt%～90wt% that in hydroisomerization catalyst, the weight content of molecular sieve is total catalyst weight, preferred 30wt%～80wt%, more preferably 40wt%～70wt%, can also contain inorganic refractory oxide in hydroisomerization catalyst, as aluminum oxide, titanium oxide, silicon oxide, boron oxide, magnesium oxide, one or more in zirconium white and clay, it is 5wt%～80wt% that inorganic refractory oxide be take final catalyzer content, be preferably 10wt%～60wt%, 15wt%～40wt% more preferably.The platinum family reactive metal can be one or more in platinum, palladium, iridium, rhodium, osmium etc., preferably contains platinum.Hydroisomerization catalyst can be seated in a reactor, also can be seated in a plurality of reactors.
In Lubricating oil base oil producing method of the present invention, can use 2～5 kinds of hydroisomerization catalysts that active metallic content is different, along the mobile direction of reaction mass, the active metallic content of hydroisomerization catalyst raises successively, every kind of catalyzer accounts for 10%～90% of total catalyst volume, is preferably 20%～80%.
The present invention, according to the characteristics of Lube basic oil material feedstocks hydroisomerizing technique, adopts the grating of suitable kind catalyzer, has improved the W-response performance.When reaction mass contacts with catalyzer, the easy reactive component in raw material is more, if catalyst activity is higher, excessive isomerization reaction and coking reaction easily occurs, unfavorable to product property, and the steady running of catalyzer is had to certain influence.Adopt the timing of different properties catalyst grade, the catalyzer that at first raw material contacts has suitable character, and easily excessive isomerization reaction does not occur reactive component, is conducive to control the side reactions such as coking yet; Along with flowing of material, during through the active high hydroisomerization catalyst of lower floor, easily reactive material is due to appropriate isomerization reaction having occurred, reactive behavior is lower than in raw material, other is difficult for iso-component, what therefore in high-activity hydrogenation heterogeneous catalyst bed, occur is mainly the isomerization reaction that is difficult for iso-component in raw material, finally show as the W-response performance and improve, and steady running is produced to Beneficial Effect.In addition, the inventive method is because used the lower catalyzer of part active metallic content, and the platinum metals price is very high, so the inventive method can obviously reduce the catalyzer cost.
Embodiment
The hydroisomerization catalyst that contains ZSM-22 molecular sieve and reactive metal Pt of below take is example, illustrates the inventive method and effect.
Contain the refractory oxide aluminum oxide in hydroisomerization catalyst, ZSM-22 molecular sieve, hydrogenation metal component Pt.10wt%～90wt% that wherein content of ZSM-22 molecular sieve is total catalyst weight, preferably 30wt%～80wt%, more preferably 40wt%～70wt%.It is 5wt%～80wt% that inorganic refractory oxide be take final catalyzer content, is preferably 10wt%～6wt%, more preferably 15wt%～40wt%.Active metal component is Pt, and the final catalyzer content of take is 0.05wt%～0.5wt%, is preferably 0.1wt%～0.4wt%.
According to conventional Nobel-metal catalyst preparation method, prepared by hydroisomerization catalyst.
(1) NaZSM-22 is exchanged into to HZSM-22, through the modifications such as dealumination complement silicon, the SiO of ZSM-22 molecular sieve
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 abundant kneading are together become to plastic paste, extruded moulding, obtain carrier through last handling processes such as super-dry, roastings.
(3) supported active metal component on carrier, by last handling processes such as drying, roastings, obtain catalyzer of the present invention.
NaZSM-22 described in step (1) first adopts ion exchange method to be exchanged into HZSM-22, and solution used 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 for keeping the pressure that solution is liquid phase, and the time is 1h～24h, Gu the liquid/mass ratio of solution and molecular sieve is 5～20.Dealumination process, solution used is acidic solution, wherein contains at least one and is selected from nitric acid, hydrochloric acid and sulfuric acid etc. mineral acid and at least one is selected from organic acid in oxalic acid, acetic acid, citric acid etc., mineral acid and organic acid mol ratio are 10: 1～1: 1, H in 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, solution used, for containing the soluble silicon compound solution, is preferably ammonium fluosilicate 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 step (2) can be selected from one or more in aluminum oxide, titanium oxide, silicon oxide, boron oxide, magnesium oxide, zirconium white and clay, is preferably aluminum oxide and/or silicon oxide, more preferably aluminum oxide.Its precursor can be selected from boehmite, pseudo-boehmite, diaspore, gibbsite and visit one or more in aluminium stone, 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, acetic acid, oxalic acid, citric acid; Extrusion aid refers to the material that is conducive to extrusion molding, is preferably sesbania powder, starch, carboxymethyl cellulose, carbon black, stone mill powder, citric acid etc.
Catalyzer described in step (3) is dry and condition roasting is as follows: 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 isomerization and production of lube base oils.
The present invention is by using the catalyzer grading loading of different bullion contents, the catalyzer classifications that activity is different are loaded, consider in raw material that at first the alkane that is easy to isomery utilize the activity of the catalyzer that activity is low, and the alkane that is difficult to isomery in raw material utilizes the activity of the catalyzer that the back activity is high, make all catalyzer in reactor can give full play to activity separately, when not reducing product property, reduce to greatest extent bullion content, thereby reduce production costs.
Below by embodiment, the present invention is further described, it does not limit use range of the present invention, and the percentage composition related to is weight percentage.
Embodiment 1
(1) processing of ZSM-22 molecular sieve
Get NaZSM-22 molecular sieve 100 grams, the ammonium nitrate solution that is 10% by 500 gram concentration, 80 ℃ of exchanges 4 hours, then repeats above-mentioned exchange once; The tartaric mixing solutions that the nitric acid that is 0.5mol/L by 800 gram volumetric molar concentrations and volumetric molar concentration are 0.2mol/L is processed 4 hours at 90 ℃; Use again 1000 gram (NH
4)
2siF
6the aqueous solution that concentration is 3% is processed 4 hours at 85 ℃, through filtering, washing, 110 ℃ of dryings 8 hours and 550 ℃ of roastings obtain the HZSM-22 of 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 then adds 270ml deionized water and 22ml concentrated nitric acid (66.5w%) abundant kneading on rolling machine, make it to become the paste plastic, extrude the cylindrical bars of diameter 1.5mm on banded extruder, 110 ℃ of dryings 8 hours, then in air atmosphere, 550 ℃ of roastings obtain carrier in 4 hours.
(3) catalyzer preparation
Get the carrier that step (2) obtains, use respectively the Pt (NH of different Pt content
4)
4cl
2solution carries out saturated dipping, and then 110 ℃ of dryings 6 hours, in air atmosphere, 500 ℃ of roastings are 4 hours, obtain respectively the catalyzer C-1 containing 0.15wt%Pt, containing the catalyzer C-2 of 0.25wt%Pt, containing the catalyzer C-3 of 0.35wt%Pt.
(4) catalyzer grating
Catalyzer C-1: catalyzer C-2: catalyzer C-3=3: 3: 4.The catalyst loading situation is in Table 1, and stock oil character is in Table 2, appreciation condition and the results are shown in Table 3.
Embodiment 2
Method for preparing catalyst is with embodiment 1, and difference is that the catalyzer grading distribution scheme is: catalyzer C-1: catalyzer C-2: catalyzer C-3=3: 5: 2.
Embodiment 3
Method for preparing catalyst is with embodiment 1, and difference is that the catalyzer grading distribution scheme is: catalyzer C-1: catalyzer C-2: catalyzer C-3=2: 3: 5.
Embodiment 4
Method for preparing catalyst is with embodiment 1, and difference is that the catalyzer grading distribution scheme is: catalyzer C-1: catalyzer C-3=5: 5.
Embodiment 5
Method for preparing catalyst is with embodiment 1, and difference is that the catalyzer grading distribution scheme is: catalyzer C-2: catalyzer C-3=5: 5.
Embodiment 6
Method for preparing catalyst is with embodiment 1, and difference is that the catalyzer grading distribution scheme is: catalyzer C-1: catalyzer C-2=5: 5.
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 C-2.
Comparative example 3
Method for preparing catalyst is with embodiment 1, and difference is a loading catalyst C-3.
Table 1 catalyst loading situation
| C-1 | C-2 | C-3 | |
| Embodiment 1 | 3 | 3 | 4 |
| Embodiment 2 | 3 | 5 | 2 |
| Embodiment 3 | 2 | 3 | 5 |
| Embodiment 4 | 5 | / | 5 |
| Embodiment 5 | / | 5 | 5 |
| Embodiment 6 | 5 | 5 | / |
| Comparative example 1 | All | / | / |
| Comparative example 2 | / | All | / |
| Comparative example 3 | / | / | All |
Table 2 stock 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, % | 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
| The catalyzer numbering | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Processing condition | |||||||||
| Reaction pressure, MPa | 9.0 | 9.0 | 9.0 | 9.0 | 9.0 | 9.0 | 9.0 | 9.0 | 9.0 |
| Volume space velocity, h -1 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Hydrogen to oil volume ratio | 800 | 800 | 800 | 800 | 800 | 800 | 800 | 800 | 800 |
| Temperature of reaction, ℃ | 320 | 320 | 320 | 320 | 320 | 320 | 320 | 320 | 320 |
| C 5 +Liquid is received, % | 94.2 | 93.7 | 94.4 | 93.6 | 95.0 | 92.5 | 94.0 | 94.8 | 94.5 |
| Product distributes | |||||||||
| C 5～130℃ | 4.4 | 3.9 | 4.2 | 3.9 | 4.0 | 3.7 | 3.9 | 4.2 | 3.8 |
| 130℃～280℃ | 3.2 | 3.4 | 3.0 | 3.3 | 3.1 | 3.2 | 2.8 | 3.7 | 2.8 |
| 280℃～350℃ | 4.9 | 4.4 | 5.4 | 5.3 | 5.5 | 5.0 | 5.8 | 5.2 | 5.2 |
| 350℃ + | 81.7 | 82.0 | 81.8 | 81.1 | 82.4 | 80.6 | 81.5 | 81.7 | 82.6 |
| 350℃ +Neutral oil character | |||||||||
| Viscosity, 40 ℃, mm 2/s | 37.57 | 38.26 | 37.53 | 36.98 | 38.56 | 37.86 | 36.45 | 38.05 | 38.12 |
| Viscosity index | 100 | 102 | 100 | 105 | 102 | 101 | 95 | 103 | 101 |
| Pour point, ℃ | -23 | -22 | -23 | -21 | -24 | -18 | -18 | -23 | -21 |
Claims (10)
1. a Lubricating oil base oil producing method, under the hydroisomerizing condition, stock oil and hydrogen are by the hydroisomerization catalyst bed, hydroisomerization catalyst comprises TON type molecular sieve and platinum metals active ingredient, in hydroisomerization catalyst, the weight content of platinum metals active ingredient is 0.05wt%～0.5wt%, it is characterized in that: described hydroisomerization catalyst bed at least comprises two kinds of hydroisomerization catalysts, press stock oil and flow hydrogen gas direction, in hydroisomerization catalyst, active metallic content increases successively.
2. in accordance with the method for claim 1, it is characterized in that: in the hydroisomerization catalyst that metal content increases successively, the weight content of hydrogenation active metals in hydroisomerization catalyst differs 0.02wt%～0.2wt%.
3. it is characterized in that in accordance with the method for claim 1: in hydroisomerization catalyst, the weight content of platinum metals active ingredient is 0.1wt%～0.4wt%.
4. in accordance with the method for claim 1, it is characterized in that: the hydroisomerizing operational condition is, reaction pressure is 1～15MPa, and temperature of reaction is 280～400 ℃, and during liquid, volume space velocity is 0.2～4h
-1, hydrogen to oil volume ratio is 100～1500.
5. in accordance with the method for claim 1, it is characterized in that: the TON type molecular sieve in hydroisomerization catalyst is one or more in ZSM-22, Nu-10, KZ-2 and ISI-1,10wt%～90wt% that in hydroisomerization catalyst, the weight content of molecular sieve is total catalyst weight.
6. in accordance with the method for claim 1, it is characterized in that: contain inorganic refractory oxide in hydroisomerization catalyst, it is 5wt%～80wt% that inorganic refractory oxide be take final catalyzer content.
7. it is characterized in that in accordance with the method for claim 6: described inorganic refractory oxide is one or more in aluminum oxide, titanium oxide, silicon oxide, boron oxide, magnesium oxide, zirconium white and clay.
8. in accordance with the method for claim 1, it is characterized in that: hydroisomerization catalyst is used 2～5 kinds of hydroisomerization catalysts that active metallic content is different, and along the mobile direction of reaction mass, the active metallic content of hydroisomerization catalyst raises successively.
9. according to the described method of claim 1 or 8, it is characterized in that: every kind of catalyzer accounts for 10%～90% of total catalyst volume.
10. it is characterized in that in accordance with the method for claim 1: the vacuum distillate that stock oil is hydrocracking tail oil, hydrotreatment or the deasphalted oil of hydrotreatment.
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| 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 |
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