CN104624215A - Distillate oil hydrofining catalyst and preparation method and application ofdistillate oil hydrofining catalyst - Google Patents
Distillate oil hydrofining catalyst and preparation method and application ofdistillate oil hydrofining catalyst Download PDFInfo
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Abstract
The invention relates to a distillate oil hydrofining catalyst and a preparation method and application ofthe distillate oil hydrofining catalyst. The distillate oil hydrofining catalyst also contains a P additive by taking gamma-Al2O3 or silicious gamma-Al2O3 as a carrier and taking Mo, Ni and/or Co, and W as active components. The distillate oil hydrofining catalyst is characterized in that based on the catalyst, the content of molybdenum trioxide is 3.0-15.0%, the content of nickel oxide and/or cobaltous oxide is 1.5-8.5%, the content of tungsten trioxide is 8.0-22.0%, the content of P2O5 is 0.5-3.5%, and the content of gamma-Al2O3 or silicious gamma-Al2O3 is 65.0-85.0%.The catalyst can be applied to the light-weight distillate oil hydrofining of reformed raw materials, gasoline distillation, coal oil distillate and the like, and has high hydrogen desulfurization activity.
Description
Technical field
The present invention relates to a kind of Hydrobon Catalyst And Its Preparation Method, more particularly, is a kind of Hydrobon catalyst and preparation method thereof about distillate particularly light ends oil.
Background technology
No. 3 jet fuel national standards (GB6537-2006) propose nearly 30 index requests from aspects such as outward appearance, color, composition, volatility, density, mobility, flammability, corrosivity, stability, cleanliness, electric conductivity, water separation index and lubricities to jet fuel.Jet fuel is one of product that in oil product, Con trolling index at most, quality requirement is the tightest.
From world wide, jet fuel is mainly produced for raw material passes through to refine with the straight run component that the boiling range cut from atmospheric distillation device is suitable, and refining link is wherein divided into again Non-adding hydrogen and hydroprocessing technique.
Non-adding hydrogen, owing to there is pollution in various degree, produces the more waste material not easily disposed, and simultaneously along with the variation of crude quality, simple Non-adding hydrogen is difficult to meet jet fuel and produces refining requirement.Non-adding hydrogen be hydroprocessed gradually technique to replace be development trend from now on.
The Main Function of hydroprocessing technique removes mercaptan, colloid and a small amount of polarity thing and pollutes impurity, reduces acid number (as removing aphthenic acids etc.).After hydrogenation, the target improvement such as smell, color, thermal oxidation stability of oil product is obvious.Because hydroconversion condition relaxes, the natural sulfide isopolarity material major part in raw material with the wear-resistant effect of antioxygen is retained, therefore the anti-oxidative stability of oil product and lubricity better.
In jet fuel unifining process, in order to retain in raw material the natural sulfide isopolarity material with antioxygen, wear-resistant effect, ensureing anti-oxidative stability and the lubricity of oil product, simultaneously in order to reduce hydrogen consumption, generally all adopting the process conditions of low temperature, low pressure, low hydrogen/gasoline ratio.On the other hand, need again to be realized mercaptan, colloid and a small amount of polarity thing in deep removal raw material and pollution impurity by hydrogenation, reduce acid number.This just requires developed catalyst, under low temperature, low pressure, low hydrogen/gasoline ratio process conditions, still have very high hydrogenation activity and activity stability, especially has very strong removal of mercaptans, depickling, improves oil product color activity.
At present, normally the light ends oil Hydrobon catalysts such as the reformed pre-hydrogenated catalyst of commercial Application or diesel oil hydrofining catalyst are directly used in jet fuel hydrogenation.Although product quality also can reach No. 3 jet fuel national standards, because the design specific aim of catalyst is not strong, there is reaction condition and relax not, the problems such as plant energy consumption is higher.
Summary of the invention
The object of this invention is to provide one and be suitable for the hydrofinishing of light ends oil, be especially suitable for the preparation method that the hydrogenation catalyst of jet fuel is produced in straight run kerosene fraction hydrofinishing.When using this catalyst treatment inferior raw material, have the advantages that operating condition relaxes.
Catalyst for hydrorefining distillate oil of the present invention, with γ-Al
2o
3or siliceous γ-Al
2o
3for carrier, with Mo, Ni and/or Co, W for active component, also containing P auxiliary agent; Take catalyst as benchmark, the content of molybdenum trioxide is 3.0 ~ 15.0%, and the content of nickel oxide and/or cobalt oxide is 1.5 ~ 8.5%, and the content of tungstic acid is 8.0 ~ 22.0%, P
2o
5content be 0.5 ~ 3.5%, γ-Al
2o
3or siliceous γ-Al
2o
3content be 65.0 ~ 85.0%.
The specific area of catalyst is 120m
2/ g ~ 190m
2/ g, pore volume 0.30ml/g ~ 0.55ml/g.Can one or more conven-tional adjuvants be contained, as Fe, Ca, Mg, Zn etc. in catalyst.
Catalyst for hydrorefining distillate oil preparation method of the present invention, comprises following process:
(1) boehmite powder and field mountain valley with clumps of trees and bamboo powder are mixed, then add the kneading such as peptizing agent, deionized water, then extrusion, drying, roasting, obtained γ-Al
2o
3or siliceous γ-Al
2o
3carrier;
(2) with the maceration extract that infusion process load contains Mo compound, prepares containing P-compound and other auxiliary agent, then dry, roasting, obtained catalyst semi-finished product.
(3) with the maceration extract that infusion process load contains W compound, prepares containing Ni and/or Co compound and auxiliary agent, then dry, roasting, obtained finished catalyst;
Dry run described in step (1) is at 100 DEG C ~ 120 DEG C dry 2h ~ 14h, and roasting process is at high temperature furnace roasting 3h ~ 8h at 500 DEG C ~ 800 DEG C.
Described in step (2) is one or both in molybdenum trioxide, ammonium molybdate containing Mo compound; Phosphorus-containing compound is one or more in ammonium dihydrogen phosphate (ADP), diammonium hydrogen phosphate, phosphoric acid, calcium phosphate, calcium monohydrogen phosphate, fatty alcohol ether phosphate, PAPE.
Dry run described in step (2) is at 100 DEG C ~ 120 DEG C dry 2h ~ 4h, and roasting process is at high temperature furnace roasting 3h ~ 8h at 450 DEG C ~ 700 DEG C.
Dry run described in step (3) is at 100 DEG C ~ 120 DEG C dry 2h ~ 4h, and roasting process is at high temperature furnace roasting 3h ~ 16h at 450 DEG C ~ 700 DEG C.
Described in above-mentioned steps (3) is one or both in nickel nitrate, basic nickel carbonate containing Ni compound; Be one or both in basic cobaltous carbonate, cobalt nitrate containing Co compound; Be ammonium metatungstate containing W compound.
The feature of the catalyst prepared by the present invention is: be first mixed with impregnation fluid carrier with Mo element and the compound of P element and the auxiliary agent of necessity, after drying and roasting, molybdenum atom with the phosphide form load of molybdenum on carrier.With the molybdenum of the existence of phosphide form, be easy to form Monolayer Dispersion at carrier surface, improve the decentralization of molybdenum.The formation of phosphide, changes the electronic structure of molybdenum, and formed act synergistically with the nickel of load in subsequent step and/or cobalt, W elements, the hydrofinishing playing catalyst is better active.
Detailed description of the invention
Content of the present invention is set forth further below in conjunction with embodiment.
Embodiment 1
(1) γ-Al
2o
3the preparation of carrier
Take 1000g without silicon boehmite powder, 30g field mountain valley with clumps of trees and bamboo powder, 30g citric acid, 3 ~ 5% dust technology 700ml mix, extruded with banded extruder, 110 DEG C of dry 10h, in air atmosphere after 650 DEG C of calcination process, obtain γ-Al
2o
3carrier.
(2) Mo-P/ γ-Al
2o
3preparation
Preparation 1000ml dipping solution: weigh 105.8g tartaric acid and join in 600ml deionized water, to stir and after being heated to 50 DEG C, weighing 157.2g ammonium molybdate (technical grade) and 28.4g ammonium dihydrogen phosphate (ADP) (technical grade) join in this solution, boil 0.5 hour, add weak aqua ammonia and solution pH value is adjusted to 4.0.After being cooled to room temperature, transferred to by solution in volumetric flask, the constant volume that adds water, to 1000ml, obtains the dipping solution containing molybdenum and phosphorus.
Take the γ-Al prepared by 500g step (1)
2o
3carrier, measures the dipping solution containing molybdenum and phosphorus that 376ml is above-mentioned prepared, incipient impregnation 30 minutes, and 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain catalyst semi-finished product.
(3) W-Ni-Mo-P/ γ-Al
2o
3the preparation of catalyst
Preparation 1000ml dipping solution: weigh 105.0g citric acid and join in 700ml water, after stirring and dissolving, weighing 242.1g nickel nitrate (technical grade) and 119.4g ammonium metatungstate (technical grade) join in this solution, boil 0.5 hour, be cooled to room temperature, transferred to by solution in volumetric flask, the constant volume that adds water, to 1000ml, obtains the dipping solution of tungstenic and nickel.
Take the Mo-P/ γ-Al prepared by 500g step (2)
2o
3catalyst semi-finished product, measure the dipping solution of above-mentioned the prepared tungstenic of 344ml and nickel, incipient impregnation 30 minutes, and 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain finished catalyst.
Embodiment 2
(1) siliceous γ-Al
2o
3the preparation of carrier
Take the siliceous boehmite of 1000g, 45g field mountain valley with clumps of trees and bamboo powder, 33g oxalic acid, 3 ~ 5% dust technology 680ml mix, extruded with banded extruder, 110 DEG C of oven dry, after the lower 550 DEG C of calcination process of air atmosphere, obtain siliceous γ-Al
2o
3carrier.
(2) the siliceous γ of Mo-P/-Al
2o
3preparation
Preparation 1000ml dipping solution: weigh 136.0g oxalic acid and join in 600ml water, to stir and after being heated to 50 DEG C, weighing 51.2g molybdenum trioxide (technical grade) and 71.3g phosphoric acid (technical grade) join in this solution, boil 0.5 hour, be cooled to room temperature, transferred to by solution in volumetric flask, the constant volume that adds water, to 1000ml, obtains the dipping solution containing molybdenum and phosphorus.
Take the siliceous γ-Al prepared by 500g step (1)
2o
3carrier, the dipping solution containing molybdenum and phosphorus measuring that 363ml prepares, incipient impregnation 30 minutes, 110 DEG C of dryings 2 hours, 500 DEG C of roastings, obtain catalyst semi-finished product.
(3) the siliceous γ of W-Ni-Mo-P/-Al
2o
3the preparation of catalyst
Maceration extract preparation is with embodiment 1 (3).
Take the siliceous γ of the Mo-P/-Al prepared by 500g step (2)
2o
3catalyst semi-finished product, measure the dipping solution of above-mentioned the prepared tungstenic of 345ml and nickel, incipient impregnation 30 minutes, and 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain finished catalyst.Embodiment 3
(1) γ-Al
2o
3the preparation of carrier
With embodiment 1 (1).
(2) Mo-P/ γ-Al
2o
3preparation
Maceration extract preparation is with embodiment 2 (2).
Take 500g γ-Al
2o
3carrier, the dipping solution containing molybdenum and phosphorus measuring that 376ml prepares, incipient impregnation 30 minutes, 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain catalyst semi-finished product.
(3) W-Ni-Mo-P/ γ-Al
2o
3the preparation of catalyst
Maceration extract preparation is with embodiment 1 (3).
Take the Mo-P/ γ-Al prepared by 500g step (2)
2o
3catalyst semi-finished product, measure the dipping solution of tungstenic that 347ml prepares and nickel, incipient impregnation 30 minutes, and 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain finished catalyst.
Comparative example 1
(1) γ-Al
2o
3the preparation of carrier
With embodiment 1 (1).
(2) W-Mo-Ni/ γ-Al
2o
3the preparation of catalyst
Configuration 1000ml dipping solution: weigh 144.0g citric acid and join in 600ml water, after stirring and dissolving, weighing 118.2g ammonium metatungstate (technical grade) and 242.0g nickel nitrate (technical grade) join in this solution, boil 1.0 hours, again 157.0g ammonium molybdate (technical grade) is joined in this solution, with concentrated ammonia liquor by solution dilution to 1000ml.Obtain the dipping solution of tungstenic, molybdenum, nickel.
Take the γ-Al prepared by 500g step (1)
2o
3carrier, measures the dipping solution of tungstenic that 375ml prepares, molybdenum, nickel, incipient impregnation 30 minutes, and 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain finished catalyst.
Comparative example 2
(1) siliceous γ-Al
2o
3the preparation of carrier
With embodiment 2 (1).
(2) the siliceous γ of W-Mo-Ni/-Al
2o
3the preparation of catalyst
Maceration extract preparation is with comparative example 1 (2).
Take the siliceous γ-Al prepared by 500g step (1)
2o
3carrier, measures the dipping solution of tungstenic that 363ml prepares, molybdenum, nickel, incipient impregnation 30 minutes, and 110 DEG C of dryings 2 hours, 460 DEG C of roastings, obtain finished catalyst.
The physico-chemical property of the catalyst above obtained by each example lists in table 1.
The composition of each routine catalyst of table 1
The evaluation of 100ml hydrogenation activity is carried out with the catalyst prepared by above each example.Evaluation result is in table 2.
The each routine catalyst activity evaluation result of table 2
| Project | Feedstock oil | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Sulphur, μ g/g | 4063 | 642 | 623 | 619 | 935 | 931 |
| Mercaptan sulfur, μ g/g | 89 | 4.5 | 4.3 | 6.1 | 26.4 | 21.2 |
| Color, number | 11 | 30 | 30 | 30 | 25 | 25 |
| Arene content, Φ % | 20.5 | 19.1 | 19.0 | 18.9 | 20.4 | 20.3 |
Note: (1) conditions of vulcanization: first catalyst uses the kerosene containing carbon disulfide 2 ω % under 290 DEG C of hydrogen atmospheres, under 7.0MPa pressure, carries out presulfurization 25h, then enters raw material; (2) reaction condition: reaction temperature 230 DEG C, pressure 2.0MPa, air speed (volume) 3.0h
-1, hydrogen oil (volume) is than 150.
Claims (7)
1. a catalyst for hydrorefining distillate oil, with γ-Al
2o
3or siliceous γ-Al
2o
3for carrier, with Mo, Ni and/or Co, W for active component, also containing P auxiliary agent, it is characterized in that: take catalyst as benchmark, the content of molybdenum trioxide is 3.0 ~ 15.0%, and the content of nickel oxide and/or cobalt oxide is 1.5 ~ 8.5%, the content of tungstic acid is 8.0 ~ 22.0%, P
2o
5content be 0.5 ~ 3.5%, γ-Al
2o
3or siliceous γ-Al
2o
3content be 65.0 ~ 85.0%.
2. a preparation method for catalyst described in claim 1, is characterized in that: comprise following process:
(1) boehmite powder and field mountain valley with clumps of trees and bamboo powder are mixed, then add the kneading such as peptizing agent, deionized water, then extrusion, drying, roasting, obtained γ-Al
2o
3or siliceous γ-Al
2o
3carrier;
(2) with the maceration extract that infusion process load contains Mo compound, prepares containing P-compound and other auxiliary agent, then dry, roasting, obtained catalyst semi-finished product.
(3) with the maceration extract that infusion process load contains W compound, prepares containing Ni and/or Co compound and auxiliary agent, then dry, roasting, obtained finished catalyst.
3. method according to claim 2, is characterized in that: the dry run described in step (1) is at 100 DEG C ~ 120 DEG C dry 2h ~ 14h, and roasting process is at high temperature furnace roasting 3h ~ 8h at 500 DEG C ~ 800 DEG C.
4. method according to claim 2, is characterized in that: described in step (2) is one or both in molybdenum trioxide, ammonium molybdate containing Mo compound; Phosphorus-containing compound is one or more in ammonium dihydrogen phosphate (ADP), diammonium hydrogen phosphate, phosphoric acid, calcium phosphate, calcium monohydrogen phosphate, fatty alcohol ether phosphate, PAPE.
5. method according to claim 2, is characterized in that: the dry run described in step (2) is at 100 DEG C ~ 120 DEG C dry 2h ~ 4h, and roasting process is at high temperature furnace roasting 3h ~ 8h at 450 DEG C ~ 700 DEG C.
6. method according to claim 2, is characterized in that: the dry run described in step (3) is at 100 DEG C ~ 120 DEG C dry 2h ~ 4h, and roasting process is at high temperature furnace roasting 3h ~ 16h at 450 DEG C ~ 700 DEG C.
7. an application for catalyst for hydrorefining distillate oil described in claim 1, is characterized in that: the hydrogenation catalyst producing jet fuel as straight run kerosene fraction hydrofinishing.
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| CN106540697A (en) * | 2015-09-22 | 2017-03-29 | 中国石油天然气股份有限公司 | Hydrogenation catalyst and preparation method thereof |
| CN107597137A (en) * | 2016-07-11 | 2018-01-19 | 中国石油天然气股份有限公司 | The preparation method of catalyst for hydrorefining distillate oil |
| CN108620108A (en) * | 2018-05-03 | 2018-10-09 | 常州大学 | A kind of preparation method of molybdenum phosphide catalyst |
| CN111318293A (en) * | 2018-12-13 | 2020-06-23 | 中国石油化工股份有限公司 | Hydrotreating catalyst for rapidly improving content of monocyclic aromatic hydrocarbon and preparation method thereof |
| WO2020135714A1 (en) * | 2018-12-28 | 2020-07-02 | 中国石油化工股份有限公司 | Pseudoboehmite, and manufacturing method therefor and application thereof |
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