CN103182310A - Method for preparing distillate oil hydrotreatment catalyst - Google Patents
Method for preparing distillate oil hydrotreatment catalyst Download PDFInfo
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- CN103182310A CN103182310A CN2011104460405A CN201110446040A CN103182310A CN 103182310 A CN103182310 A CN 103182310A CN 2011104460405 A CN2011104460405 A CN 2011104460405A CN 201110446040 A CN201110446040 A CN 201110446040A CN 103182310 A CN103182310 A CN 103182310A
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Abstract
The invention relates to a method for preparing a distillate oil hydrotreatment catalyst. Ni, Co, W/Mo active components are loaded by gamma-Al2O3 or silicon-containing gamma-Al2O3, P element is included as a cocatalyst component, and any element selected from the group consisting of Mg, Zn, Fe and Ca may also be included as a cocatalyst component. The method for preparing the distillate oil hydrotreatment catalyst comprises the following steps: (1) firstly preparing gamma-Al2O3 or a silicon-containing gamma-Al2O3 carrier; (2) loading the gamma-Al2O3 or the silicon-containing gamma-Al2O3 with a Ni metal component and a P auxiliary component, then drying and calcining; (3) soaking the carrier obtained in step (2) into a solution of Co-containing compound, and W and/or Mo-containing compound, drying and calcining to obtain a finished catalyst. The catalyst can be used for hydrotreatment of light distillate oils such as a reforming raw material, gasoline fraction and kerosene fraction, and has a high hydrodesulfurization activity.
Description
Technical field
The present invention relates to a kind of hydrogenization catalyst preparation method, more particularly, is a kind of about the distillate preparation method of the Hydrobon catalyst of light ends oil particularly.
Background technology
No. 3 jet fuel national standards (GB 6537-2006) have proposed nearly 30 index requests from aspects such as outward appearance, color, composition, volatility, density, flowability, flammability, corrosivity, stability, cleanliness, electric conductivity, water separation index and lubricities to jet fuel.Jet fuel is one of product that the control index at most in the oil product, quality requirement is the tightest.
From world wide, jet fuel mainly is, and to be raw material with the suitable straight run component of boiling range that cuts from the atmospheric distillation device produce by refining, and refining link wherein is divided into non-hydrogenation technique and hydroprocessing technique again.
Non-hydrogenation technique is because existence pollution in various degree produces the waste material of more difficult disposal, and along with the variation of former oil quality, simple non-hydrogenation technique is difficult to satisfy the refining requirement of jet fuel production simultaneously.It is from now on development trend that non-hydrogenation technique is replaced by hydroprocessing technique gradually.
The main effect of hydroprocessing technique is to remove mercaptan, colloid and small amount of polar thing and pollute impurity, reduces acid number (as removing aphthenic acids etc.).Indexs such as the smell of oil product, color, thermal oxidation stability are improved obviously behind the hydrogenation.Because hydroconversion condition relaxes, the natural sulfide isopolarity material major part that has the wear-resistant effect of antioxygen in the raw material obtains keeping, so the anti-oxidative stability of oil product and lubricity are better.
In the jet fuel unifining process, in order to keep the natural sulfide isopolarity material that has antioxygen, wear-resistant effect in the raw material, guarantee anti-oxidative stability and the lubricity of oil product, in order to reduce the hydrogen consumption, generally all adopt the process conditions of low temperature, low pressure, low hydrogen/gasoline ratio simultaneously.On the other hand, need again to realize mercaptan, colloid and the small amount of polar thing in the deep removal raw material and pollute impurity by hydrogenation, reduce acid number.This just requires the catalyst developed, still has very high hydrogenation activity and activity stability under low temperature, low pressure, low hydrogen/gasoline ratio process conditions, especially has very strong removal of mercaptans, depickling, improves oil product color activity.
At present, normally light ends such as the reformed pre-hydrogenated catalyst of commercial Application or diesel oil hydrofining catalyst oil Hydrobon catalyst is directly used in the jet fuel hydrogenation.Though product quality also can reach the jet fuel national standard No. 3, because the catalyst design specific aim is not strong, exists reaction condition and relax inadequately, problem such as plant energy consumption is higher.
Summary of the invention
The purpose of this invention is to provide a kind of light ends oil hydrofinishing that is suitable for, especially be suitable for the refining hydrogenization catalyst preparation method of producing jet fuel of virgin kerosene cut fraction hydrogenation.When using this catalyst treatment inferior raw material, have the advantages that operating condition relaxes.
Light ends oil Hydrobon catalyst of the present invention is with γ-Al
2O
3Or siliceous γ-Al
2O
3Being carrier, is active component with Ni, Co and W and/or Mo, also contains the P auxiliary agent, is that absolutely nickel oxide is 1.5%~5.5% in the catalyst weight, and cobalt oxide is 0.5%~3.5%, and tungstic acid and/or molybdenum trioxide are 12.0%~22.0%, P
2O
5Be 0.5%~3.5%, γ-Al
2O
3Or siliceous γ-Al
2O
3Be surplus.
The specific area of catalyst is 120m
2/ g~190m
2/ g, pore volume 0.30ml/g~0.55ml/g.Can contain one or more conventional auxiliary agents in the catalyst, as Mg, Zn, Fe, Ca etc.
The concrete preparation process of light ends oil Hydrobon catalyst of the present invention is:
(1) gets siliceous or not siliceous boehmite powder, adding field mountain valley with clumps of trees and bamboo powder mixes, adding peptizing agent, deionized water again mixes and pinches until becoming plastic shape, at 100 ℃~120 ℃ dry 2h~14h, in 500 ℃~800 ℃ following roasting 3h~8h, the programming rate of roasting is 1 ℃/min~3 ℃/min in high temperature furnace.
(2) contain the Ni compound with the equi-volume impregnating dipping, contain the maceration extract that P-compound and other auxiliary agent are prepared, soaked carrier is at 100 ℃~120 ℃ dry 2h~4h, in high temperature furnace in 450 ℃~700 ℃ following roasting 3h~8h, the programming rate of roasting is 1 ℃/min~3 ℃/min, makes the catalyst semi-finished product.
(3) contain C o compound with the equi-volume impregnating dipping, contain the maceration extract that W and/or Mo compound and other auxiliary agent are prepared, soaked carrier is at 100 ℃~120 ℃ dry 2h~4h, in high temperature furnace in 450 ℃~700 ℃ following roasting 3h~16h, the programming rate of roasting is 1 ℃/min~3 ℃/min, makes the catalyst finished product.
The Ni compound that contains described in the above-mentioned steps (2) is in nickel nitrate, the basic nickel carbonate one or both; 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, the PAPE.
The Co compound that contains described in the above-mentioned steps (3) is in basic cobaltous carbonate, the cobalt nitrate one or both; Containing the W compound is ammonium metatungstate; Contain the Mo compound and be in ammonium molybdate, the molybdenum trioxide one or both.
The characteristics of the catalyst that the present invention is prepared are: at first compound and the necessary auxiliary agent with Ni element and P element is mixed with the maceration extract impregnated carrier, and after drying and the roasting, nickle atom loads on the carrier with the phosphide form of nickel.With the nickel that exists of phosphide form, be easy to form individual layer at carrier surface and disperse, improved the decentralization of nickel.The formation of phosphide has changed the electronic structure of nickel, forms synergy with the cobalt element of load in the subsequent step, brings into play the effect as adjuvant component better, has improved the catalytic activity of tungsten and/or molybdenum.
The specific embodiment
Further set forth content of the present invention below in conjunction with embodiment.
Embodiment 1
(1) γ-Al
2O
3The preparation of carrier
Take by weighing the no silicon boehmite powder, 30g field mountain valley with clumps of trees and bamboo powder, 30g citric acid of 1000g, rare nitric acid 700ml of 3~5% mixes, and uses the banded extruder extrusion modling, 110 ℃ of dry 10h after 650 ℃ of calcination process, obtain γ-Al under air atmosphere
2O
3Carrier.
(2) Ni-P/ γ-Al
2O
3Preparation
Preparation 1000ml dipping solution: weighing 107.6g tartaric acid joins in the 600ml deionized water, after stirring and being heated to 50 ℃, weighing 83.6g nickel nitrate (technical grade) and 26.3g ammonium dihydrogen phosphate (ADP) (technical grade) join in this solution, boiled 0.5 hour, and added weak aqua ammonia solution p H value is transferred to 4.0.After being cooled to room temperature, solution is transferred in the volumetric flask, added the water constant volume to 1000ml, obtain nickeliferous and dipping solution phosphorus.
Take by weighing the prepared γ-Al of 500g step (1)
2O
3Carrier is measured the dipping solution of the above-mentioned nickeliferous and phosphorus of preparing of 375ml, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 ℃ of roastings obtain the catalyst semi-finished product.
(3) Co-Mo-Ni-P/ γ-Al
2O
3Preparation of catalysts
Preparation 1000m l dipping solution: weighing 105.0g citric acid joins in the 700ml water, after the stirring and dissolving, weighing 49.3g basic cobaltous carbonate (technical grade) and 266.0g ammonium molybdate (technical grade) join in this solution, boiled 0.5 hour, be cooled to room temperature, solution is transferred in the volumetric flask, added the water constant volume to 1000ml, obtain containing the dipping solution of cobalt and molybdenum.
Take by weighing the prepared Ni-P/ γ-Al of 500g step (2)
2O
3The catalyst semi-finished product are measured the above-mentioned dipping solution of preparing that contains cobalt and molybdenum of 347ml, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 roastings obtain the catalyst finished product.
Embodiment 2
(1) siliceous γ-Al
2O
3The preparation of carrier
Take by weighing the siliceous boehmite, 45g field mountain valley with clumps of trees and bamboo powder, 35g oxalic acid of 1000g, rare nitric acid 680m l of 3~5% mixes, and uses the banded extruder extrusion modling, 110 ℃ of oven dry after the following 550 ℃ of calcination process of air atmosphere, obtain siliceous γ-Al
2O
3Carrier.
(2) the siliceous γ-Al of Ni-P/
2O
3Preparation
Preparation 1000ml dipping solution: weighing 140.0g oxalic acid joins in the 600ml water, after stirring and being heated to 50 ℃, weighing 45.5g basic nickel carbonate nickel (technical grade) and 31.3g calcium monohydrogen phosphate (technical grade) join in this solution, boiled 0.5 hour, be cooled to room temperature, solution is transferred in the volumetric flask, added the water constant volume to 1000ml, obtain nickeliferous and dipping solution phosphorus.
Take by weighing the prepared siliceous γ-Al of 500g step (1)
2O
3Carrier is measured the dipping solution of the nickeliferous and phosphorus that 366m l prepares, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 500 roastings obtain the catalyst semi-finished product.
(3) the siliceous γ-Al of Co-Mo-Ni-P/
2O
3Preparation of catalysts
The maceration extract preparation is with embodiment 1 (3).
Take by weighing the prepared siliceous γ-Al of Ni-P/ of 500g step (2)
2O
3The catalyst semi-finished product are measured the above-mentioned dipping solution of preparing that contains cobalt and molybdenum of 340ml, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 roastings obtain the catalyst finished product.
Embodiment 3
(1) γ-Al
2O
3The preparation of carrier
With embodiment 1 (1).
(2) Ni-P/ γ-Al
2O
3Preparation
The maceration extract preparation is with embodiment 2 (2).
Take by weighing 500g γ-Al
2O
3Carrier is measured the dipping solution of the nickeliferous and phosphorus that 375ml prepares, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 ℃ of roastings obtain the catalyst semi-finished product.
(3) Co-Mo-Ni-P/ γ-Al
2O
3Preparation of catalysts
The maceration extract preparation is with embodiment 1 (3).
Take by weighing the prepared Ni-P/ γ-Al of 500g step (2)
2O
3The catalyst semi-finished product are measured the dipping solution that contains cobalt and molybdenum that 347ml prepares, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 ℃ of roastings obtain the catalyst finished product.
Comparative example 1
(1) γ-Al
2O
3The preparation of carrier
With embodiment 1 (1).
(2) Co-Mo-Ni/ γ-Al
2O
3Preparation of catalysts
Configuration 1000ml dipping solution: weighing 144.0g citric acid joins in the 600ml water, after the stirring and dissolving, weighing 44.0g basic cobaltous carbonate (technical grade) and 119.0g nickel nitrate (technical grade) join in this solution, boiled 1.0 hours, again 272.0g ammonium molybdate (technical grade) is joined in this solution, with concentrated ammonia liquor solution is diluted to 1000ml.Obtain containing the dipping solution of cobalt, molybdenum, nickel.
Take by weighing the prepared γ-Al of 500g step (1)
2O
3Carrier is measured the dipping solution that contains cobalt, molybdenum, nickel that 375ml prepares, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 ℃ of roastings obtain the catalyst finished product.
Comparative example 2
(1) siliceous γ-Al
2O
3The preparation of carrier
With embodiment 2 (1).
(2) the siliceous γ-Al of Co-Mo-Ni/
2O
3Preparation of catalysts
The maceration extract preparation is with comparative example 1 (2).
Take by weighing the prepared siliceous γ-Al of 500g step (1)
2O
3Carrier is measured the dipping solution that contains cobalt, molybdenum, nickel that 366ml prepares, incipient impregnation 30 minutes, and 110 ℃ of dryings 2 hours, 460 ℃ of roastings obtain the catalyst finished product.
More than the physico-chemical property of each routine prepared catalyst list in table 1.
The composition of each routine catalyst of table 1
Carry out the evaluation of 100m l hydrogenation activity with the prepared catalyst of above each example.Evaluation result sees Table 2.
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, g/g | 4071 | 742 | 683 | 699 | 1035 | 1131 |
Mercaptan sulfur, g/g | 83 | 4.7 | 5.3 | 6.1 | 28.4 | 31.2 |
Color, number | 13 | 30 | 30 | 30 | 25 | 25 |
Arene content, Φ % | 20.7 | 19.1 | 19.0 | 18.9 | 20.4 | 20.3 |
Annotate: (1) conditions of vulcanization: catalyst is at first used the kerosene that contains carbon disulfide 2% under 290 hydrogen atmospheres, under 7.0MPa pressure, carry out presulfurization 25h, advances raw material then; (2) reaction condition: reaction temperature 230, pressure 2.0MPa, air speed (volume) 3.0h
-1, hydrogen oil (volume) is than 150.
Claims (5)
1. the preparation method of a catalyst for hydrogenation of fraction oil is characterized in that: with γ-Al
2O
3Or siliceous γ-Al
2O
3Being carrier, is active component with Ni and Co and W and/or Mo, contains the P auxiliary agent, and in catalyst weight percentage, nickel oxide is 1.5%~5.5%, and cobalt oxide is 0.5%~3.5%, and tungstic acid and/or molybdenum trioxide are 12.0%~22.0%, P
2O
5Content be 0.5%~3.5%, γ-Al
2O
3Or siliceous γ-Al
2O
3Be surplus;
(1) boehmite powder and field mountain valley with clumps of trees and bamboo powder are mixed, add peptizing agent, deionized water again and mix and pinch, extrusion, drying, roasting make γ-Al then
2O
3Or siliceous γ-Al
2O
3Carrier;
(2) contain the Ni compound with the infusion process load, contain the maceration extract that P-compound and other auxiliary agent are prepared, dry, roasting makes the catalyst semi-finished product then;
(3) contain the Co compound with the infusion process load, contain the maceration extract that W and/or Mo compound and other auxiliary agent are prepared, dry, roasting makes the catalyst finished product then.
2. the preparation method of catalyst for hydrogenation of fraction oil according to claim 1, it is characterized in that: the dry run described in the step (1) is at 100 ℃~120 ℃ dry 2h~14h, and roasting process is in 500 ℃~800 ℃ following roasting 3h~8h at high temperature furnace.
3. the preparation method of catalyst for hydrogenation of fraction oil according to claim 1 is characterized in that: the Ni compound that contains described in the step (2) is in nickel nitrate, the basic nickel carbonate one or both; 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, the PAPE.
4. the preparation method of catalyst for hydrogenation of fraction oil according to claim 1, it is characterized in that: the dry run described in the step (2) is at 100 ℃~120 ℃ dry 2h~4h, and roasting process is in 450 ℃~700 ℃ following roasting 3h~8h at high temperature furnace.
5. the preparation method of catalyst for hydrogenation of fraction oil according to claim 1, it is characterized in that: the dry run described in the step (3) is at 100 ℃~120 ℃ dry 2h~4h, and roasting process is in 450 ℃~700 ℃ following roasting 3h~16h at high temperature furnace.
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Cited By (11)
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CN103638987A (en) * | 2013-12-02 | 2014-03-19 | 煤炭科学研究总院 | Hydrogenation catalyst carrier for coal liquefaction oil, catalyst as well as preparation method and application of hydrogenation catalyst carrier |
WO2015067583A1 (en) * | 2013-11-07 | 2015-05-14 | Shell Internationale Research Maatschappij B.V. | Process for preparing a hydrotreating catalyst |
CN104624215A (en) * | 2013-11-15 | 2015-05-20 | 中国石油天然气股份有限公司 | Distillate oil hydrofining catalyst and preparation method and application ofdistillate oil hydrofining catalyst |
CN105478129A (en) * | 2014-09-17 | 2016-04-13 | 中国石油化工股份有限公司 | Hydrotreatment catalyst and application thereof |
CN105478156A (en) * | 2014-09-17 | 2016-04-13 | 中国石油化工股份有限公司 | Hydrotreatment catalyst and application thereof |
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 |
CN106914260A (en) * | 2015-12-24 | 2017-07-04 | 中国石油天然气股份有限公司 | Oil hydrogenation catalyst for refining, its preparation method and application |
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 |
CN109647452A (en) * | 2017-10-10 | 2019-04-19 | 中国石油化工股份有限公司 | Prepare the hydrogenation catalyst of cyclohexylamine |
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 |
CN115069253A (en) * | 2022-07-14 | 2022-09-20 | 西安交通大学 | Antioxidant organic coated nickel-based catalyst and preparation method and application thereof |
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CN105478156A (en) * | 2014-09-17 | 2016-04-13 | 中国石油化工股份有限公司 | Hydrotreatment catalyst and application thereof |
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