CN101942321A - Method for producing base oil of lubricating oil by isomerization dewaxing - Google Patents
Method for producing base oil of lubricating oil by isomerization dewaxing Download PDFInfo
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Abstract
The invention discloses a method for producing the base oil of lubricating oil by isomerization dewaxing. Under hydroisomerization condition, crude oil and hydrogen pass through a hydroisomerization catalyst bed; a hydroisomerization catalyst comprises a TON type molecular sieve and 0.05 to 0.5 weight percent of active ingredients of platinum group metals; the hydroisomerization bed at least comprises two hydroisomerization catalysts; and along the flow direction of the crude oil and the hydrogen, the molecular sieve content of the hydroisomerization catalysts is sequentially increased. The method of the invention has the advantages of adjusting the components of the catalyst, improving the comprehensive reaction performance, maximally reducing the molecular sieve content and reducing the production cost at the same time of ensuring the activity of a reaction system.
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 height, 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 because a large amount of macromolecular cpds is converted into small-molecule substance, make base oil yield low, the viscosity index loss is big, by product is worth 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, is subjected to paying close attention to greatly and having many documents and patent report.
At present a lot of about the report of isomerization dewaxing catalyst, for example, U.S. Pat P5990371,5833837,5817907,5149421,5135638,5110445,4919788,4419420,4601993,5699162,4518485 etc. has 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.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.With the n-dodecane is raw material, and transformation efficiency is～85%, isomerization selectivity～75%.
Isomerization dewaxing is to adopt the dual-function catalyst with special pore structure to make high-melting-point 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.
At present these lubricant base production technologies adopt same active catalyzer to carry out isomerization reaction mostly, do not take into full account that differential responses zone material properties changes whole reaction system combined reaction Effect on Performance under the response behaviour.
Summary of the invention
At the deficiencies in the prior art, the present invention proposes a kind of production method of lube base oil, is guaranteeing the active while of reaction system, adjusts catalyzer and forms, and improves the combined reaction performance, reduces molecular sieve content to greatest extent, reduces production costs.
The method that isomerization dewaxing of the present invention is produced lubricant base 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, the weight content of platinum metals active ingredient is 0.05wt%～0.5wt% in the hydroisomerization catalyst, be preferably 0.1wt%～0.4wt%, described hydroisomerization catalyst bed comprises two kinds of hydroisomerization catalysts at least, increases successively by the molecular sieve content of stock oil and flow hydrogen gas direction hydroisomerization catalyst catalyzer.In the hydroisomerization catalyst that molecular sieve content increases successively, the weight content of adjacent hydroisomerization catalyst molecular sieve differs 5wt%～25wt%.
In the lube base oil producing method of the present invention, stock oil can be the various suitable stock oils in this area, owing to use the platinum metals to be reactive metal, generally need remove impurity such as sulphur, nitrogen in the stock oil, as 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 as 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, can use 2～5 kinds of hydroisomerization catalysts that molecular sieve content is different, along the mobile direction of reaction mass, the molecular sieve content of hydroisomerization catalyst raises successively, every kind of hydroisomerization catalyst accounts for 10%～90% of total hydroisomerization catalyst volume, is preferably 20%～80%.Active metallic content in the hydroisomerization catalyst also can be different, and the hydroisomerization catalyst active metallic content that preferred molecular sieve content is high is higher, with the different hydroisomerization catalyst of coupling molecular sieve content.
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 contains 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%, the molecular sieve content of the various hydroisomerization catalysts that molecular sieve content is different is all in above-mentioned scope.Can also contain inorganic refractory oxide in the hydroisomerization catalyst, as in aluminum oxide, titanium oxide, silicon oxide, boron oxide, magnesium oxide, zirconium white and the clay one or more, inorganic refractory oxide is 5wt%～80wt% in final catalyzer content, be 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.Hydroisomerization catalyst can be seated in the reactor, also can be seated in a plurality of reactors.
The present invention adopts the grating of suitable kind catalyzer 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, excessive isomerization reaction and coking reaction took place easily, and is unfavorable to product property, and the steady running of catalyzer is had certain influence.Adopt the timing of different properties catalyst grade, the catalyzer that raw material at first contacts has suitable character, and easily excessive isomerization reaction does not take place reactive component, helps controlling side reactions such as coking yet; Along with flowing of material, during through the active high hydroisomerization catalyst of lower floor, easily appropriate isomerization reaction owing to taken place in reactive material, reactive behavior is lower than that other is difficult for iso-component in the raw material, what therefore take place in high-activity hydrogenation heterogeneous catalyst bed 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 lower catalyzer of part molecular sieve content, and the molecular sieve price is higher, so the inventive method can suitably reduce the catalyzer cost.
Embodiment
The present invention considers the alkane isomerization complexity difference of different chain length, and the sequencing catalyzer grading loading different, that activity is different of their generation isomerization reactions, gives full play to activity separately.
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%.
Catalyzer of the present invention 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 the carrier by 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, citric acid 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, magnesium oxide, 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, gibbsite 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 citric acid; Extrusion aid is meant the material that helps extrusion molding, is preferably sesbania powder, starch, carboxymethyl cellulose, carbon black, stone mill powder, citric acid etc.
The condition dry and roasting of catalyzer described in the step (3) 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 differing molecular sieve content, the catalyzer classification filling that activity is different, consider that the alkane that is easy to isomery in the raw material at first utilizes active low activity of such catalysts, and the alkane that is difficult to isomery in the raw material utilizes the active high activity of such catalysts in back, make all catalyzer in the reactor can both give full play to separately activity, when not reducing product property, reduce molecular sieve content to greatest extent, thereby reduce production costs.
Below by embodiment the present invention is further specified, it does not limit use range of the present invention, and the percentage composition that relates to is a weight percentage.
The processing of embodiment 1ZSM-22 molecular sieve
Getting NaZSM-22 molecular sieve 100 gram, is that 10% ammonium nitrate solution exchanges 4 hours at 80 ℃ with 500 gram concentration, repeats above-mentioned exchange then once; With 800 gram volumetric molar concentrations is that the nitric acid of 0.5mol/L and tartaric mixing solutions that volumetric molar concentration is 0.2mol/L were handled 4 hours at 90 ℃; 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.
The preparation of embodiment 2 carriers
Get HZSM-22 molecular sieve 65 grams of embodiment 1 preparation, pseudo-boehmite (butt 72%) 28 grams, SB powder (butt 72%) 21 grams, sesbania powder 2 grams, mix, add 30ml deionized water and 2.5ml 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 D-1 (molecular sieve account for final support of the catalyst weight 65%) in 4 hours in air atmosphere then
Get HZSM-22 molecular sieve 50 grams of embodiment 1 preparation, pseudo-boehmite (butt 72%) 42 grams, SB powder (butt 72%) 28 grams, sesbania powder 2 grams, mix, add 40ml deionized water and 2.5ml 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 D-2 (molecular sieve account for final support of the catalyst weight 50%) in 4 hours in air atmosphere then
Get HZSM-22 molecular sieve 40 grams of embodiment 1 preparation, pseudo-boehmite (butt 72%) 48 grams, SB powder (butt 72%) 35 grams, sesbania powder 2 grams, mix, add 50ml deionized water and 2.5ml 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 D-3 (molecular sieve account for final support of the catalyst weight 40%) in 4 hours in air atmosphere then
Embodiment 3 Preparation of Catalyst
Get carrier D-1, D-2 and the D-3 of embodiment 2 preparations, use Pt (NH respectively
4)
4Cl
2Solution carries out saturated dipping, and then 110 ℃ of dryings 6 hours, 500 ℃ of roastings are 4 hours in air atmosphere, obtain catalyzer C-1 respectively, catalyzer C-2, and catalyzer C-3 contains Pt 0.3% by weight in the catalyzer.
Embodiment 4
Catalyst grade prescription case is: catalyzer C-3: catalyzer C-2: catalyzer C-1=3: 3: 4.
Embodiment 5
Catalyst grade prescription case is: catalyzer C-3: catalyzer C-2: catalyzer C-1=3: 5: 2.
Embodiment 6
Catalyst grade prescription case is: catalyzer C-3: catalyzer C-2: catalyzer C-1=2: 3: 5.
Embodiment 7
Catalyst grade prescription case is: catalyzer C-3: catalyzer C-1=5: 5.
Embodiment 8
Catalyst grade prescription case is: catalyzer C-3: catalyzer C-2=5: 5.
Embodiment 9
Catalyst grade prescription case is: catalyzer C-2: catalyzer C-1=5: 5.
Comparative example 1
Catalyst grade prescription case is: complete loading catalyst C-3.
Comparative example 2
Catalyst grade prescription case is: complete loading catalyst C-2.
Comparative example 3
Catalyst grade prescription case is: complete loading catalyst C-1.
Catalyzer C-1, catalyzer C-2, specifically filling situation of catalyzer C-3 sees Table 1.Estimate stock oil character and see Table 2, appreciation condition and the results are shown in Table 3.
Table 1 catalyst loading situation
| C-3 | C-2 | C-1 | |
| Embodiment 4 | 3 | 3 | 4 |
| Embodiment 5 | 3 | 5 | 2 |
| Embodiment 6 | 2 | 3 | 5 |
| Embodiment 7 | 5 | / | 5 |
| Embodiment 8 | 5 | 5 | / |
| Embodiment 9 | / | 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, 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
Claims (10)
1. an isomerization dewaxing is produced the method for lubricant base, comprise 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, the weight content of platinum metals active ingredient is 0.05wt%～0.5wt% in the hydroisomerization catalyst, it is characterized in that: described hydroisomerization catalyst bed comprises two kinds of hydroisomerization catalysts at least, increases successively by the molecular sieve content of stock oil and flow hydrogen gas direction hydroisomerization catalyst.
2. according to the described method of claim 1, it is characterized in that: the TON type molecular sieve that comprises in the hydroisomerization catalyst is one or more among ZSM-22, SSZ-32, Nu-10, KZ-2 and the ISI-1.
3. according to claim 1 or 2 described methods, it is characterized in that: in the hydroisomerization catalyst that molecular sieve content increases successively, the weight content of molecular sieve in hydroisomerization catalyst differs 5wt%～25wt%.
4. ask 1 described method according to right, it is characterized in that: the weight content of TON type molecular sieve is the 10wt%～90wt% of total catalyst weight in the hydroisomerization catalyst.
5. it is characterized in that in accordance with the method for claim 1: the weight content of TON type molecular sieve is the 30wt%～80wt% of total catalyst weight in the hydroisomerization catalyst.
6. in accordance with the method for claim 1, it is characterized in that: use 2～5 kinds of hydroisomerization catalysts that molecular sieve content is different, along the mobile direction of reaction mass, the molecular sieve content of hydroisomerization catalyst raises successively, and every kind of hydroisomerization catalyst accounts for 10%～90% of total hydroisomerization catalyst volume.
7. it is characterized in that in accordance with the method for claim 6: every kind of hydroisomerization catalyst accounts for 20%～80% of total hydroisomerization catalyst volume.
8. in accordance with the method for claim 1, it is characterized in that: the hydroisomerizing operational condition is that 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.
9. in accordance with the method for claim 1, it is characterized in that: contain inorganic refractory oxide in the hydroisomerization catalyst, inorganic refractory oxide is 5wt%～80wt% in final hydroisomerization catalyst weight content.
10. it is characterized in that in accordance with the method for claim 1: stock oil is the vacuum distillate of hydrocracking tail oil, hydrotreatment or the deasphalted oil of hydrotreatment.
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| CN107286982B (en) * | 2016-04-05 | 2019-03-22 | 中国石油化工股份有限公司 | A kind of preparation method of lube base oil |
| CN108102698A (en) * | 2016-11-25 | 2018-06-01 | 中国石油化工股份有限公司 | A kind of method for producing lube base oil |
| CN108102698B (en) * | 2016-11-25 | 2020-07-03 | 中国石油化工股份有限公司 | Method for producing lubricating oil base oil |
| CN106964398B (en) * | 2017-03-09 | 2019-07-02 | 武汉凯迪工程技术研究总院有限公司 | Hydroisomerizing dewaxing catalyst and preparation method thereof |
| CN106964398A (en) * | 2017-03-09 | 2017-07-21 | 武汉凯迪工程技术研究总院有限公司 | Hydroisomerizing dewaxing catalyst and preparation method thereof |
| CN111073696A (en) * | 2018-10-18 | 2020-04-28 | 中国海洋石油集团有限公司 | Method for reducing cloud point of base oil of high-viscosity lubricating oil and base oil of lubricating oil |
| CN111073696B (en) * | 2018-10-18 | 2022-03-01 | 中国海洋石油集团有限公司 | Method for reducing cloud point of base oil of high-viscosity lubricating oil and base oil of lubricating oil |
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