CN1184707A - Catalyst for hydrogenation of fraction oil, and method for preparing same - Google Patents

Catalyst for hydrogenation of fraction oil, and method for preparing same Download PDF

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CN1184707A
CN1184707A CN96120875A CN96120875A CN1184707A CN 1184707 A CN1184707 A CN 1184707A CN 96120875 A CN96120875 A CN 96120875A CN 96120875 A CN96120875 A CN 96120875A CN 1184707 A CN1184707 A CN 1184707A
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catalyst
carrier
hours
solution
oil
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CN1060097C (en
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王致善
李坚
夏国富
扈林杰
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Sinopec Research Institute of Petroleum Processing
China Petrochemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petrochemical Corp
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Abstract

The component of the catalyst consists of active components Ni, W and Co, the component of the auxiliary catalyst is P or the mixture of P and Mg, the carrier is gama-Al2O3. Said catalyst is used for hydrogenation of fraction oil meanwhile it possesses of higher activities of hydrodesulfurization and hydrodenitrification. The prepn. method is simple and the strength of the made catalyst is fairly high.

Description

A kind of catalyst for hydrogenation of fraction oil and preparation method thereof
The present invention relates to hydrocarbon hydrogenizing treamtent catalyst, more particularly, is a kind of about the particularly hydrodesulfurization, hydrodenitrogenation catalyst and preparation method thereof of light ends oil and intermediate oil of distillate.
Hydrofinishing is petroleum refining industry method commonly used, and its main purpose is sulphur, nitrogen, oxygen compound or the metal of removing in the petroleum hydrocarbon etc.For example the raw material naphtha used of reformer generally must carry out pre-hydrogenation before entering the reforming reaction system, to remove wherein the catalyst harmful substance, comprises sulphur, nitrogen and other impurity.For other distillate such as kerosene, diesel oil distillate, for guaranteeing product quality, often need hydrofinishing, remove wherein sulphur, nitrogen and aromatic hydrocarbons etc., to improve smoke point and diesel index etc.The used catalyst of hydrogenation process plays an important role to hydrogenation, and the catalyst that above-mentioned fraction oil hydrogenation refining is commonly used adopts γ-Al more 2O 3, also sneak into SiO sometimes 2Representative catalyst used for hydrogenation of distilled oil fraction is that trade names are the catalyst of S-12, and it is a kind of Co-Mo/Al 2O 3The type catalyst, be used for the pre-hydrogenation of reforming raw oil, have higher desulphurizing activated, but reaction temperature and pressure are higher, at least 310 ℃ of reaction temperatures, the minimum 2.5MPa of pressure (China Petrochemical Corporation's production and operation coordination portion is compiled, " oil refining process units basic data compilation; fuel oil part ", 1994).
In recent years, for adapting to the protection environment requirement, reported many and had high desulfurization, denitrogenation and take off the catalyst used for hydrogenation of distilled oil fraction of aromatic hydrocarbons activity, phosphorous catalyst is exactly one of them.The introduction of US5135902 patent be a kind of be the load hydrogenation catalyst of active component with Ni, W, P, its carrier is the bunge bedstraw herb shape bar with narrow pore-size distribution (60～80A accounts for 85%) of drying, 625 ± 30 ℃ of roastings.The arene saturating activity of this catalyst all is significantly increased than conventional Ni-W catalyst and Ni-Mo-P catalyst.The US5472595 patent also is the hydrocarbons hydrogenation catalyst of a kind of Ni-W-P, the catalyst that provides in the example is that the active component of nickeliferous ≈ 7%, tungsten＞35%, phosphorus＞1% was immersed on the active carbon through two steps or three steps, and the catalyst that this catalyst takes off the Ni-W/ carbon that the aromatic hydrocarbons specific activity do not phosphorate is high by 78%.Above-mentioned two kinds of catalyst all have the higher aromatic hydrocarbons activity of taking off, but hydrodesulfurization, hydrodenitrogenationactivity activity do not improve.
EP0482817A 1Mo-Ni-P or Co-Mo-P hydrogenization catalyst preparation method have been reported, it is with the complexing agent of hydroxycarboxylic acid as the reactive metal element, with its metering join in the co-impregnated solution of reactive metal element and phosphoric acid, carrier impregnation is in wherein, can make catalyst being lower than 200 ℃ of dryings.This catalyst has higher desulphurizing activated.Decomposition for fear of complex compound, the strict control of needs baking temperature when preparing this catalyst, and this catalyst is the same with the described catalyst of US5472595, without roasting, active element exists with salt or complex form, be subjected to the influence of environment such as water, temperature bigger, poor stability is unfavorable for preserving and long-distance transport.
The purpose of this invention is to provide a kind ofly have simultaneously that high alkene is saturated, the catalyst for hydrogenation of fraction oil of hydrodesulfurization and hydrodenitrogeneration.
Another object of the present invention provides a kind of simple and can obtain high-intensity Preparation of catalysts method.
Catalyst of the present invention is to be active component with W, Ni, Co, and the mixture of P or P and Mg is as co-catalyst component.The composition content of following catalyst is that the weight with catalyst is benchmark, and metallic element is in oxide form, and concrete content is as follows: WO 310～30%, NiO1.0～7.0%, CoO0.01～1.0%, co-catalyst component MgO0.1～5.0%, P0.3～5.0%, optimum content: active component WO 316～27%, NiO1.5～4.0%, CoO0.02～0.3%, co-catalyst component MgO0.5～4.0%, P0.5～4.0%, all the other are γ-Al 2O 3
Described γ-Al 2O 3Precursor is selected from any in unformed aluminium oxide, false boehmite, boehmite, gibbsite, the surge aluminium stone, a preferably false diaspore and boehmite, gama-alumina aperture 50～100 account for more than 90%, and carrier adopts special-shaped bar, preferably cloverleaf pattern.
Described catalyst routinely method before use carries out presulfurization.
Preparation of catalysts method of the present invention comprises the following steps;
(1) γ-Al 2O 3Precursor is through moulding, drying, and 500～700 ℃ of roastings 1～6 hour under the existence of air or water vapour again make γ-Al 2O 3, (2) are with γ-Al 2O 3Soak in the compound water solution that P that immersion prepares or P and Mg mix, filtration, drying 400～700 ℃ of following roastings 2～8 hours, obtain containing the γ-Al of co-catalyst component then 2O 3Carrier, the γ-Al that contains co-catalyst component that (3) obtain (2) step 2O 3In the compound water solution that contains W, Ni, Co that the carrier impregnation intervention prepares earlier, filtration, drying promptly obtained catalyst prod in 2～5 hours 400～600 ℃ of following roastings then.
Described active component Co can add in (2) step, makes the γ-Al that contains Co and co-catalyst component 2O 3
Described co-catalyst component P can make the aqueous solution with active component Ni, W, Co and flood γ-Al again in (3) step 2O 3Or contain γ-Al of Mg 2O 3
Above-mentioned preparation process (2), (3) step can also adopt the saturated dipping method in hole.
Described Ni, W, Co compound water solution make according to a conventional method, and wherein the compound of Ni, Co element is nitrate, acetate, carbonate, subcarbonate, preferably nitrate, subcarbonate.
Described P, Mg compound water solution make according to a conventional method, and the compound of Mg is a magnesium nitrate, and the aqueous solution of P is phosphoric acid, metaphosphoric acid or its esters.
Catalyst of the present invention can be used for saturated, the hydrodenitrogeneration hydrodesulfurization of alkene of reforming prerefining feedstock oil, gasoline fraction and intermediate oil, and its operating condition can be adjusted in following ranges according to feedstock oil character with to the requirement of oil quality: 200～400 ℃ of reaction temperatures, volume space velocity 3～15h -1, hydrogen dividing potential drop 0.8～6.0MPa, hydrogen/oil 50～800: 1 (body).
Major advantage of the present invention: owing to adopt Ni-W and micro-Co as main active component, and obtain best proportioning, introduce P again as co-catalyst component, adjust the performance of catalyst, therefore catalyst of the present invention is used for the distillate hydrogenation processing, can have high hydrodesulfurization and hydrodenitrogenationactivity activity simultaneously, as be mixed with the reformer feed of the triumph coker gasoline of 2.5% (body), can under low pressure, low hydrogen/gasoline ratio and high-speed condition, produce qualified reformer feed in addition, owing to introduce P, also increased the hydrogenation aromatics-removing activity of catalyst.
Preparation of catalysts method of the present invention is simple, and used raw material all is commercially available prod, and the catalyst strength of acquisition is than higher.
Further specify characteristics of the present invention with example below.
Example 1
This example is the carrier of preparation catalyst.
In the false boehmite powder that 200g Shandong Aluminum Plant produces, add 7.0g sesbania powder, mix.Take by weighing that the 7.0g citric acid is measured 1.4ml nitric acid and water is made into 130ml solution, this solution under agitation is added in the compound powder, pinch through mixing, to make D be the wet bar of 1.6mm cloverleaf pattern to extrusion.This extrudate is down put into the steam treatment stove after dry 3 hours at 120 ℃ and is handled, and than 1: 1, constant temperature 6 hours made carrier a in 550 ℃, aqua.Carrier a specific surface 202M 2/ g, pore volume 0.39ml/g can a few aperture 64 , intensity 20.2N/mm.
Example 2
This example is the γ-Al that contains P with the boehmite preparation 2O 3Carrier.
In the boehmite powder that 150g Wenzhou catalyst plant is produced, add 4.5g sesbania powder, mix.4.5g citric acid, 14.8g85% phosphoric acid and 1ml nitric acid water are made into 105ml solution, this solution slowly is added in the mixed powder, constantly stir, pinch through mixing then, extrusion makes D=1.6mm cloverleaf pattern bar.Should wet bar 140 ℃ dry 2 hours down, 580 ℃ of following roastings 3 hours make carrier b.Carrier b specific surface 180m 2/ g, pore volume 0.37ml/g can a few aperture 66 , intensity 30.0N/mm.
Example 3
This example is to prepare γ-Al with boehmite 2O 3Carrier.
Boehmite powder 400g and 12g sesbania powder with Wenzhou catalyst plant production mix.16g citric acid and 3.2ml nitric acid water are made into 300ml solution.Solution is mixed with powder, and warp mixes and pinches, extrusion, makes D=1.6mm cloverleaf pattern bar.Should wet bar 120 ℃ of dryings 4 hours, 600 ℃ of roastings 4 hours make carrier c.Carrier specific surface 190m 2/ g, pore volume 0.40ml/g can a few aperture 90 , intensity 26N/mm.
Example 4
This example is preparation Ni-W-Co/Al 2O 3-P catalyst.Concrete preparation process:
(1) takes by weighing 7.95g85%H 3PO 4Be made into 43ml solution with water, with hole saturation dipping 50g carrier a3 hour, then 120 ℃ of dryings 2 hours, 560 ℃ of roastings 4 hours made phosphorous γ-Al with this solution 2O 3Carrier.
(2) with 0.12g cobalt nitrate, 4.91g nickel nitrate, ammonium metatungstate (hereinafter to be referred as AMT) solution (concentration 77.6gWO 3/ 100ml) 13.5ml is made into 45ml solution.The phosphorous carrier that makes by (1) step with hole saturation dipping with this solution 3 hours, then 120 ℃ dry 2 hours down, 420 ℃ of following roastings 4 hours make catalyst A.
Example 5
This example is preparation Ni-W-Co/Al 2O 3-P-Mg catalyst.Concrete preparation process:
(1) adds water with 85% phosphatase 11 .95g, magnesium nitrate 124g and be made into 43ml solution.With hole saturation dipping 50g carrier a3 hour, then 120 ℃ of dryings 2 hours, 570 ℃ of roastings 4 hours made the γ-Al that contains P-Mg with this solution 2O 3Carrier.
(2) get 0.13g cobalt nitrate, 9.53g nickel nitrate and AMT solution (concentration such as example 4) 20.8ml, add water and be made into the 42ml co-impregnated solution.With above-mentioned same method dipping 50g by (1) step make contain the P-Mg carrier, drying, roasting make catalyst B.
Example 6
This example is preparation Ni-W-Co/Al 2O 3-P catalyst.
Get 0.12g cobalt nitrate, 5.61g nickel nitrate and 1.72ml AMT solution (concentration 73gWO 3/ 100ml), water dissolving is made into the 32ml co-impregnated solution, and with this solution impregnation 40g carrier b4 hour, then 110 ℃ of dryings 3 hours down, 440 ℃ of following roastings 4 hours made catalyst C.
Example 7
This example is preparation Ni-W-Co/Al 2O 3-P catalyst.
(1) takes by weighing 10.7g85%H 3PO 4Be made into 44ml solution with water.With this solution impregnation 50g carrier c3 hour, then 120 ℃ dry 2 hours down, 570 ℃ of following roastings 4 hours make and contain the P carrier.
(2) take by weighing 0.30g cobalt nitrate, 7.62g nickel nitrate and 23.5ml AMT solution (concentration 73gWO 3/ 100ml), water dissolving is made into the 39ml co-impregnated solution, and with the above-mentioned carrier that is made by (1) step of the saturated dipping of this solution 4 hours, then 120 ℃ of dryings 3 hours down, 420 ℃ of following roastings 4 hours made catalyst D.
Example 8
This example is preparation Ni-W-Co/Al 2O 3-P catalyst.Concrete preparation process:
(1) weighing 85% phosphoric acid 5.79g, water is made into the 51ml phosphoric acid solution.Phosphoric acid solution was added among the 60g carrier c dipping 3 hours, and wet bar drying and roasting get phosphorous carrier.
(2) take by weighing cobalt nitrate 0.12g, nickel nitrate 5.50g, measure AMT solution 24.2ml (concentration such as example 6) and be made into co-impregnated solution 52ml with water.By the phosphorous carrier that makes of (1) step 4 hours, wet bar drying, roasting made catalyst D with this solution impregnation 62.5g.
Example 9
This example is according to EP0,482, and 817A 1The catalyst that example 13 makes in the patent application is called comparative example 1.
Use the dry glue powder (Al (OH) that Chang Ling, Hunan oil-refining chemical factory catalyst plant is sold in Chang Ling in this comparative example 1 3Powder) as support material.Concrete preparation process:
(1) adds 3g sesbania powder in the dry glue powder of 100g Chang Ling, mix.Measure 3.5ml nitric acid, 4.0g citric acid, water is made into 95ml solution.Solution is mixed with powder, and warp mixes and pinches, extrusion is made the wet bar of D=1.6mm cloverleaf pattern.This extrudate is 120 ℃ of dryings 3 hours, and 600 ℃ of roastings 4 hours make carrier.After measured, this carrier specific surface 261m 2/ g, pore volume 0.63ml/g, with EP0,482,817A 1Patent application example 13 used carrier character are close.
(2) take by weighing 7.7g molybdenum oxide, 3.24g nickelous carbonate, 2.46g85% phosphoric acid, add water, heating for dissolving is made into the 38ml co-impregnated solution.The carrier that is made by (1) step with co-impregnated solution dipping 40g 4 hours, the wet bar behind the dipping made comparative example 1 catalyst down in dry 5 hours through 115 ℃.
The catalyst property of above-mentioned example 4～example 9 is listed in table 1.
Example 10
This example is mixed 2.5v% triumph coker gasoline with grand celebration direct steaming gasoline and grand celebration direct steaming gasoline catalyst A, B, C, D is carried out activity rating, and compares with comparative example 1 and comparative example 2 activity of such catalysts.
The catalyst activity evaluation is carried out in the 50ml fixed bed reactors, and hydrogen once passes through.Must presulfurization handle before the evaluating catalyst.Sulfurized oil is to contain 2%CS 2Direct steaming gasoline.Conditions of vulcanization is respectively:
Comparative example 1 catalyst:
Sulfide stress 1.6MPa, hydrogen to oil volume ratio 300: 1, volume space velocity 2.0h -1, be warming up to 130 ℃ by 30～50 ℃/h during sulfuration and advance sulfurized oil, rise to 260 ℃ by 80 ℃/h then, constant temperature 1 hour, 60 ℃/h are warming up to 350 ℃, constant temperature 5 hours, sulfuration finishes.
Other catalyst:
Sulfide stress 1.6MPa, hydrogen to oil volume ratio 300: 1, volume space velocity 2.0h -1, be warming up to 150 ℃ by 30～50 ℃/h during sulfuration and advance sulfurized oil, rise to 230 ℃ by 50 ℃/h then, constant temperature 3 hours rises to 290 ℃ with same programming rate then, constant temperature 3 hours, sulfuration finishes.
Change into to estimate after the sulfuration end and use feedstock oil, under reaction condition, need stablize and to begin to estimate activity through 24～30 hours.The data that all logical oil of each catalyst activity running in 100 hours post analysis obtains.
Estimate and list in table 2 with feedstock oil character.The catalyst activity evaluation result is listed in table 3.
As can be seen from Table 3, the catalyst made from the inventive method, under high-speed, low hydrogen/gasoline ratio, low pressure and lower temperature, no matter use direct steaming gasoline, still with the low grade oils that contains a certain amount of nitrogen and colloid, sulphur and nitrogen can be reduced to below the 0.5ppm fully, meet the catalytic reforming feedstock requirement, its activity is apparently higher than the comparative example catalyst.In addition, the aromatic hydrogenation performance of the catalyst made from the inventive method is compared with comparative example, and raising is also arranged.
Table 1 catalyst property [notes]
[notes] comparative example 2 catalyst are that the trade mark of being produced by Uop Inc. is the catalyst of S-12, and its character is measured result.
Table 2 feedstock oil character
Table 3 catalyst activity result of the test [notes] [notes] reaction condition: reaction pressure 1.6MPa, volume space velocity 10h -1, hydrogen to oil volume ratio 90: 1.

Claims (7)

1. a hydrocarbon hydrogenizing treamtent catalyst is characterized in that forming and contains active constituent Ni, W, Co, and the co-catalyst composition is selected from P or P and Mg mixture, and carrier is γ-Al 2O 3, specifically form content (is benchmark with the catalyst weight): WO 310～30%, NiO1.0～7.0%, CoO0.01～1.0%, P0.3～5.0%, MgO0.1～5.0%, all the other are γ-Al 2O 3
2. according to the described catalyst of claim 1, it is characterized in that WO 316～27%, NiO1.5～4.0%, CoO0.02～0.3%, P0.5～4.0%, MgO0.05～4.0%.
3. the described Preparation of catalysts method of claim 1 is characterized in that preparation process and condition comprise (1) γ-Al 2O 3Precursor is through moulding, drying, and 500～700 ℃ of roastings 1～6 hour under the existence of air or water vapour again make γ-Al 2O 3, (2) are with γ-Al 2O 3Soak in the compound water solution that P that immersion prepares or P and Mg mix, filtration, drying 400～700 ℃ of following roastings 2～8 hours, obtain containing the γ-Al of co-catalyst component then 2O 3γ-the Al that contains co-catalyst component that carrier (3) obtains (2) step 2O 3Carrier impregnation is in the compound water solution that contains W, Ni, Co, and filtration, drying promptly made catalyst in 2～5 hours 400～600 ℃ of following roastings then.
4. in accordance with the method for claim 3, it is characterized in that active component Co can adding be mixed with the aqueous solution with co-catalyst component P in (2) step, floods γ-Al again 2O 3
5. in accordance with the method for claim 3, it is characterized in that co-catalyst component P can make the aqueous solution with active component Ni, W, Co and flood γ-Al again in (3) step 2O 3Or contain γ-Al of Mg 2O 3
6. in accordance with the method for claim 3, it is characterized in that described γ-Al 2O 3Precursor is selected from any in unformed aluminium oxide, false boehmite, boehmite, gibbsite, the surge aluminium stone, γ-Al 2O 3Aperture 50～100 account for more than 90% of total pore volume.
7. the described catalyst of claim 1 is characterized in that can be used for the hydrotreatment process of reforming prerefining feedstock oil, gasoline fraction and intermediate oil.
CN96120875A 1996-12-11 1996-12-11 Catalyst for hydrogenation of fraction oil, and method for preparing same Expired - Lifetime CN1060097C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101808732B (en) * 2007-08-06 2013-08-14 国际壳牌研究有限公司 Composition useful in the catalytic hydroprocessing of hydrocarbon feedstocks, method of making such catalyst, and process of using such catalyst
CN103521236A (en) * 2013-10-11 2014-01-22 中国海洋石油总公司 Preparation method of hydrofining catalyst for high-activity coker gasoline
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 and application thereof
CN109647450A (en) * 2017-10-10 2019-04-19 中国石油化工股份有限公司 Hydrogenation catalyst for synthesizing cyclohexane 1 amine

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1006202B (en) * 1984-05-18 1989-12-27 国际壳牌研究有限公司 Process for preparing supported hydroconversion catalysts and catalysts thus prepared
CN1019502B (en) * 1989-12-11 1992-12-16 中国石油化工总公司抚顺石油化工研究院 Hydrofined catalyst and preparing process thereof
US5068025A (en) * 1990-06-27 1991-11-26 Shell Oil Company Aromatics saturation process for diesel boiling-range hydrocarbons
US5472595A (en) * 1994-08-09 1995-12-05 Texaco Inc. Process for hydrodearomatization of hydrocarbon oils using carbon supported metal sulfide catalysts promoted by phosphate

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101808732B (en) * 2007-08-06 2013-08-14 国际壳牌研究有限公司 Composition useful in the catalytic hydroprocessing of hydrocarbon feedstocks, method of making such catalyst, and process of using such catalyst
CN103521236A (en) * 2013-10-11 2014-01-22 中国海洋石油总公司 Preparation method of hydrofining catalyst for high-activity coker gasoline
CN103521236B (en) * 2013-10-11 2015-08-19 中国海洋石油总公司 A kind of method for making of high activity coking gasoline hydrogenation refining 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 and application thereof
CN109647450A (en) * 2017-10-10 2019-04-19 中国石油化工股份有限公司 Hydrogenation catalyst for synthesizing cyclohexane 1 amine

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