CN102039140A - Heavy oil hydrotreating catalyst as well as preparation method and application thereof - Google Patents
Heavy oil hydrotreating catalyst as well as preparation method and application thereof Download PDFInfo
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- CN102039140A CN102039140A CN2009102042703A CN200910204270A CN102039140A CN 102039140 A CN102039140 A CN 102039140A CN 2009102042703 A CN2009102042703 A CN 2009102042703A CN 200910204270 A CN200910204270 A CN 200910204270A CN 102039140 A CN102039140 A CN 102039140A
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Abstract
The invention discloses a heavy oil hydrotreating catalyst as well as a preparation method and application thereof. The heavy oil hydrotreating catalyst comprises aluminium oxide and raw clay, wherein the raw clay accounts for 0.5-30 wt% of the catalyst. The heavy oil hydrotreating catalyst is prepared by using a full kneading method. The hydrogenation activity metal components are added in the form of salt solutions. The heavy oil hydrotreating catalyst is suitable for the processes of heavy oil hydrodesulfurization, hydrodenitrogenation and hydrogenation carbon residue removal, has favorable service performance, and especially has outstanding property of hydrogenation carbon residue removal.
Description
Technical field
The present invention relates to a kind of hydrocarbon raw material hydrotreating catalyst and its production and application, relate in particular to a kind of heavy oil hydrogenation conversion catalyst and its production and application.
Background technology
Contain impurity such as a large amount of heavy metal (as nickel, vanadium), sulphur, nitrogen in the heavy oil (as the decompression residuum of the reduced crude of crude oil, crude oil, heavy crude, oil-sand, synthetic heavy oil product etc.); and colloid and bitum content are higher; in order to satisfy the requirement of catalytic cracking charging; the protection downstream catalyst; these impurity must be removed as much as possible, and hydrotreatment is the optimum technology that removes above-mentioned impurity.Heavy oil hydrogenating treatment catalyst generally comprises protective agent, catalyst for demetalation, desulphurization catalyst, reforming catalyst etc. by the function of use branch.The main effect of reforming catalyst is exactly sulphur, nitrogen and the carbon residue etc. that remove to greatest extent through in demetalization and the desulfurizing agent material.In addition, in the heavy-oil hydrogenation processing procedure, because furol viscosity height and impurity content are big, therefore the air speed of heavy-oil hydrogenation processing procedure is very little, so catalyst consumption quite other oil refining process increases greatly, and heavy oil hydrogenating treatment catalyst is short service life, and recyclability is poor, and the cost that therefore reduces catalyst is particularly important.
The cost of catalyst is made of expense of raw materials and producing cost.For developing cheap catalyst, can use from the reduction raw material expense on the one hand and start with, but must guarantee that the serviceability of catalyst is unaffected.As everyone knows, clay is a kind of important nonmetal mineral resource, and it has many valuable practical values and manufacturability, is the indispensable raw mineral materials of many departments therefore.China is the country that abounds with clay, and the great deal of raw materials reserves are arranged, and price is very cheap.For petroleum chemical industry, it is sial that clay is mainly formed, and can make full use of clay and prepare heavy oil hydrogenating treatment catalyst.But the surface area of clay and pore volume are very little, the activated centre number seldom, it is very little to do catalyst activity with it separately, must and activated alumina use jointly.But the suitable preliminary treatment of needs usually just can reach the serviceability requirement when natural clay was used for catalysis material.
What reduce the catalyst cost is exactly to reduce producing cost on the other hand, and producing cost has bigger difference because of the difference of production method.At present, the preparation of hydrotreating catalyst mainly contains methods such as coprecipitation, infusion process, kneading method.Coprecipitation consumes more, and the reactive metal utilization rate is low, operating influence factor complexity, and preparation repeatability is not good enough.Infusion process adopts twice oven dry and roasting (process first drying and roasting during the carrier moulding), and manufacturing cost is higher.Kneading method preparation technology is simple, and is with short production cycle, the efficient height, and cost is low.But its shortcoming is that the aperture of catalyst is more because sintering temperature is subjected to certain limitation, and the aperture is less, and intensity is relatively poor.
US5089453 adopts kneading method to prepare residual oil hydrocatalyst, adopts to add acid solution earlier in its preparation process, adds the alkaline solution neutralization then, uses a large amount of TiCl simultaneously
4Make improvements agent, the titaniferous amount is higher in the catalyst, because TiCl
4Hydrolytic process easily produces harmful fog, makes will use specialized apparatus in the production process, and the production technology more complicated, the production difficulty is big, and security is low, and cost is higher.And for the preparation after catalyst also to flood again with phosphorus-containing compound solution, just obtain final catalyst, this makes the preparation process complexity again, has increased production cost.
US6387248 adopts dried kneading method to prepare residual oil hydrocatalyst, and with phosphorus as auxiliary agent.Join in the alumina powder because metal is the form with metal salt powder, cause the intensity of active metal component skewness and catalyst also relatively poor relatively easily.
CN1448468A discloses a kind of mink cell focus and hydrotransforming catalyst for residual oil and preparation method thereof, it is support material that catalyst adopts a kind of siliceous aluminium oxide, the preparation process of siliceous aluminium oxide adopts in becoming the glue process and adds minor amount of silicon, the silicon of adding surplus can make this aluminium oxide have desirable pore structure when having more strong acid center after becoming glue or in the ageing process.The acidity of catalyst of this method preparation has improved, but the cost in silicon source is higher and preparation process is complicated.
US4443558 adopts complete kneading method one-step shaping to prepare catalyst.Do not introduce any auxiliary agent in its catalyst, Preparation of catalysts adopts and adds acid solution earlier, the method that adds the alkaline solution neutralization then, this method is because acid solution and the aluminium oxide effect that adds earlier is stronger, make that pore volume, the specific surface loss of aluminium oxide are serious, the performance of final catalyst is unsatisfactory.
CN99113299.8 discloses a kind of high activity residual oil hydrogenation conversion catalyst and preparation method thereof.Method for preparing catalyst is to adopt complete kneading method,, as auxiliary agent aluminum hydroxide solid elastomer powder and molecular sieve is mixed by a certain percentage with titanium, adds the alkaline solution of group vib metal then earlier, adds the acid solution of VIII family and/or group vib metal again.The pore volume of preparation catalyst is 0.36～0.60ml/g, and specific surface is 190～280m
2/ g.The performance that makes of this catalyst needs further to improve, and particularly residual oil takes off the carbon residue performance needs further to improve.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of active height and the low heavy oil hydrogenating treatment catalyst of preparation cost are provided, another object of the present invention provides above-mentioned Preparation of catalysts methods and applications.
Heavy oil hydrogenating treatment catalyst of the present invention comprises aluminium oxide, clay original soil (original soil of non-modified) and hydrogenation activity component, and its medium clay soil original soil is with SiO
2Meter accounts for the 0.5wt%～30wt% of catalyst weight, is preferably 1wt%～25wt%, and heavy oil hydrogenating treatment catalyst adopts full kneading method preparation.When full kneading method prepared catalyst, the hydrogenation active metals component added with the form of salting liquid.
The active hydrogenation metal of heavy oil hydrogenating treatment catalyst of the present invention contains MoO by weight
3Or WO
3Be 1.0wt%～20wt%, be preferably 5.0wt%～15.0wt%, CoO or NiO are 0.5wt%～10.0wt%, are preferably 1.0wt%～5.0wt%.Specific surface area of catalyst is 120～290m
2/ g is preferably 180～240m
2/ g, pore volume is 0.35～0.66ml/g, is preferably 0.44～0.58ml/g, and pore volume and specific area are measured with the nitrogen low-temperature adsorption, and infrared acidity is measured by the chemisorbed pyridine method.
Catalyst of the present invention is applied to hydrodesulfurization, hydrodenitrogeneration and the removal of ccr by hydrotreating process of heavy oil, and optimum is used for the hydrodenitrogeneration and the removal of ccr by hydrotreating process of heavy oil.Above-mentioned hydrodesulfurization, hydrodenitrogeneration and removal of ccr by hydrotreating process conditions can adopt the process conditions of this area routine.
Heavy oil hydrogenating treatment catalyst preparation method of the present invention comprises:
(1) aluminum hydroxide solid elastomer powder and above-mentioned clay are formed required ratio mixing in catalyst, add the salting liquid that contains reactive metal, mix and pinch evenly, become plastic;
(2) by the moulding on former of (1) gained material;
(3) descended dry 1～5 hour at 80～120 ℃ by (2) gained material, or adopt air dry;
(4) by (3) gained material under 300～800 ℃, roasting 1～6 hour.
Required aluminum hydroxide solid elastomer powder is commercially available aluminum hydroxide solid elastomer powder, and this dry glue powder can be converted into γ-Al 450 ℃～850 ℃ roastings
2O
3, can contain suitable auxiliary agent in the aluminum hydroxide solid elastomer powder, as titanium, phosphorus, silicon etc.
The described clay of step (1) is one or more in the clays such as kaolin, imvite, diatomite, natural clay, the SiO of clay
2/ Al
2O
3The molecule mol ratio is 1～80, and the clay consumption is with SiO
2Meter accounts for the 0.5wt%～30.0wt% of catalyst weight.
Can also add expanding agent and/or extrusion aid etc. as required in the step (1).Described expanding agent is for being physics expanding agent such as carbon black, ammonium carbonate, polyvinyl alcohol, starch etc., its consumption is counted 0.5wt%～10wt% with total aluminium oxide in the material, also can be chemical enlargement agent such as phosphoric acid, boric acid etc., its consumption is counted 0.5wt%～5wt% with total aluminium oxide in the material, also can be their mixture.Described extrusion aid is the sesbania powder, and it is 1wt%～5wt% that its consumption is counted with total aluminium oxide in the material.Contain the reactive metal salting liquid and be the solution that contains VIII family and/or group vib metal with the conventional method preparation, wherein VIII family metal is Co or Ni, and the group vib metal is Mo or W.The inventive method is used, and to contain the active metal salt stability of solution good, under the less situation of solution usage, can make metal obtain good dispersion effect.
In general, when being used to prepare catalyst, clay need carry out the preliminary treatment modification in advance, the application is by discovering, after will comprising the material and hydrogenation active metals salt solution mix of clay original soil, the hydrogenation active metals component enters in the former soil structure of clay, and in the roasting process of its rear catalyst, change of properties has taken place the clay original soil that contains active metal component, this change of properties helps the heavy-oil hydrogenation processing procedure, particularly takes off the carbon residue effect and improves obviously.
The preparation method of catalyst for hydrotreatment of residual oil of the present invention adopts the simple full kneading method of process, adding cheap raw clay simultaneously reduces production cost greatly, and, introduce siliceous clay, the more especially macropore of hydrodesulfurization of heavy-oil hydrogenation that is suitable for can not only be provided, and increased the acid amount of catalyst, and then increased the cracking performance of catalyst.In addition, cooperate the special reactive metal salting liquid of forming, optimized the character of catalyst, the serviceability, particularly residual hydrogenation that have improved catalyst are taken off the carbon residue performance and are obviously improved.
The specific embodiment
Technical essential of the present invention comprises: the one, in catalyst preparation process, add siliceous natural clay, and promptly reduced the catalyst cost, increased the acid amount of catalyst again.The 2nd, reactive metal is that the form with solution once joins in the powder, plays the modifying function to the clay original soil simultaneously.Catalyst has experienced primary drying and roasting among the present invention, has reduced operating procedure, has shortened the production cycle, helps reducing the catalyst manufacturing cost.
Further describe technical characterictic of the present invention below in conjunction with embodiment, but be not limited to embodiment.
Embodiment 1
Take by weighing commercially available aluminum hydroxide solid elastomer powder (water content 25wt%) 100 grams, take by weighing SiO again
2/ Al
2O
3Be that 1.2 kaolin original soil, 10.8 grams, carbon black 1.6 grams, extrusion aid sesbania powder 1.6 grams and 100ml contain the reactive metal salting liquid, 5ml distilled water.Above-mentioned mixing of materials is even, make plastic, on banded extruder, be extruded into the cylinder bar then, drying is 2 hours under 110 ℃, then 700 ℃ of following roastings 3 hours, gets catalyst A.Wherein contain ammonium molybdate and basic nickel carbonate in the reactive metal salting liquid, content is pressed MoO
3Count 10wt% and count 2wt%, obtain catalyst A by NiO.
Embodiment 2
In embodiment 1, change kaolin into 54.9 grams, carbon black 5.1 grams, extrusion aid sesbania powder 2.0 grams and 109ml and contain the reactive metal salting liquid, 10ml distilled water obtains catalyst B.
Embodiment 3
In embodiment 1, change kaolin into 173.5 grams, carbon black 8.1 grams, extrusion aid sesbania powder 3.2 grams and 138ml and contain the reactive metal salting liquid, 13ml distilled water gets catalyst C.
Embodiment 4
In embodiment 1, change kaolin into SiO
2/ Al
2O
3Be that 65 imvite, 6.1 grams, carbon black 3.9 grams, extrusion aid sesbania powder 1.6 grams and 100ml contain the reactive metal salting liquid, 5ml distilled water, catalyst D.
Embodiment 5
In embodiment 1, change kaolin into SiO
2/ Al
2O
3Be that 6.7 carclazyte, 7.2 grams, carbon black 3.9 grams, extrusion aid sesbania powder 1.6 grams and 100ml contain the reactive metal salting liquid, 5ml distilled water, catalyst E.
Embodiment 6
In embodiment 1, change kaolin into SiO
2/ Al
2O
3Be that 77 diatomite, 5.7 grams, carbon black 3.9 grams, extrusion aid sesbania powder 1.6 grams and 100ml contain the reactive metal salting liquid, 5ml distilled water, catalyst F.
Comparative example 1
This comparison example is the catalyst for preparing by the method that CN99113299.8 describes.
Take by weighing the aluminum hydroxide solid elastomer powder identical 100 grams, SiO with embodiment 1
2/ Al
2O
3Be 5.6 molecular sieve, 19.3 grams, add ammonium molybdate solution 110 gram, wherein MoO
3Concentration is 14%, and it is wetting with aluminium hydrate powder to be fully mixed to alkali lye, adds 119 gram acid solutions then, wherein contains NiCl
24.4%, fully mix to pinch to become to mix and pinch body, extruded moulding, drying is 4 hours under 100 ℃, then 490 ℃ of following roastings 3 hours, obtains catalyst G.
Comparative example 2
According to embodiment 1 described method, wherein the kaolin original soil was made metakaolin in 2 hours 900 ℃ of roastings in advance, other method is identical with embodiment 1, obtains catalyst H.
Embodiment 7
This example provides the physico-chemical property of above each routine institute controlling catalyst, sees Table 1.
The physico-chemical property of table 1 different catalysts
With autoclave prepared catalyst is carried out activity rating, the feedstock oil character of evaluation sees Table 2.Appreciation condition is: raw material oil mass: 210ml, and catalytic amount: 70ml, temperature: 410 ℃, pressure: 14.5MPa, reaction time 60min.That estimates the results are shown in Table 3.
Table 2 feedstock oil character
| Project | Data |
| Density (20 ℃)/gcm -1 | 0.973 |
| S/wt％ | 2.22 |
| N/μg·g -1 | 2899 |
| Ni+V/μg·g -1 | 241.78 |
| CCR/wt％ | 14.2 |
Table 3 evaluating catalyst result
As seen from Table 3, the performance of catalyst of the present invention is better than the comparative catalyst, especially takes off the carbon residue performance and obviously is better than the comparative catalyst; Demetalization, desulfurization and nitrogen removal performance and comparative catalyst are suitable.
Claims (10)
1. heavy oil hydrogenating treatment catalyst, it is characterized in that: heavy oil hydrogenating treatment catalyst comprises aluminium oxide, clay original soil and hydrogenation activity component, its medium clay soil original soil accounts for the 0.5wt%～30wt% of catalyst weight, and heavy oil hydrogenating treatment catalyst adopts full kneading method preparation.
2. according to the described catalyst of claim 1, it is characterized in that: the clay original soil accounts for the 1wt%～25wt% of catalyst weight.
3. according to the described catalyst of claim 1, it is characterized in that: heavy oil hydrogenating treatment catalyst contains hydrogenation activity component MoO by weight
3Or WO
3Be 1.0wt%～20wt%, CoO or NiO are 0.5wt%～10.0wt%, and specific surface area of catalyst is 120～290m
2/ g, pore volume are 0.35～0.66ml/g.
4. according to the described catalyst of claim 1, it is characterized in that: the clay original soil is one or more in kaolin, imvite, diatomite and the natural clay.
5. the preparation method of the described heavy oil hydrogenating treatment catalyst of claim 1, it is characterized in that: process comprises:
(1) aluminum hydroxide solid elastomer powder and above-mentioned clay are formed required ratio mixing in catalyst, add the salting liquid that contains reactive metal, mix and pinch evenly, become plastic;
(2) by the moulding on former of (1) gained material;
(3) descended dry 1～5 hour at 80～120 ℃ by (2) gained material, or adopt air dry;
(4) by (3) gained material under 300～800 ℃, roasting 1～6 hour.
6. it is characterized in that in accordance with the method for claim 5: the aluminum hydroxide solid elastomer powder is for can be converted into γ-Al 450 ℃～850 ℃ roastings
2O
3The aluminum hydroxide solid elastomer powder.
7. in accordance with the method for claim 5, it is characterized in that: the described clay of step (1) is one or more in kaolin, imvite, diatomite and the natural clay, the SiO of clay
2/ Al
2O
3The molecule mol ratio is 1～80, and the clay consumption is counted 0.5wt%～30.0wt% by catalyst weight.
8. it is characterized in that in accordance with the method for claim 5: step also adds expanding agent and/or extrusion aid in (1).
9. in accordance with the method for claim 5, it is characterized in that: containing the reactive metal salting liquid is the solution that contains VIII family and/or group vib slaine, and wherein VIII family metal is Co or Ni, and the group vib metal is Mo or W.
10. the application of the described heavy oil hydrogenating treatment catalyst of claim 1 in heavy oil hydrodesulfurization, hydrodenitrogeneration and removal of ccr by hydrotreating process.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015007230A1 (en) | 2013-07-18 | 2015-01-22 | 中国石油大学(北京) | Iron-based hydrogenation catalyst and applications thereof |
| CN104646006A (en) * | 2013-11-22 | 2015-05-27 | 中国石油天然气股份有限公司 | Load type hydrodenitrogeneration catalyst and preparation method thereof |
| CN104826584A (en) * | 2015-04-22 | 2015-08-12 | 芜湖市鸿坤汽车零部件有限公司 | Multi-plant modified composite active carbon particle with devulcanization effect and preparation method thereof |
| CN106925285A (en) * | 2015-12-29 | 2017-07-07 | 中国石油天然气股份有限公司 | Heavy-oil hydrogenation catalyst and preparation method thereof |
| CN108144626A (en) * | 2017-11-27 | 2018-06-12 | 南京工业大学 | A kind of lamellar composite type Hydrobon catalyst and preparation method |
| CN108404897A (en) * | 2017-02-10 | 2018-08-17 | 中国石油天然气股份有限公司 | A kind of catalyst carrier for hydrgenating heavy oil, preparation method, using its catalyst and catalyst preparation method |
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| CN1434744A (en) * | 1999-12-21 | 2003-08-06 | 格雷斯公司 | Hydrothermally stable high pore volume aluminum oxide/swellable clay composites and methods of thein preparation and use |
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2009
- 2009-10-21 CN CN2009102042703A patent/CN102039140A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1434744A (en) * | 1999-12-21 | 2003-08-06 | 格雷斯公司 | Hydrothermally stable high pore volume aluminum oxide/swellable clay composites and methods of thein preparation and use |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015007230A1 (en) | 2013-07-18 | 2015-01-22 | 中国石油大学(北京) | Iron-based hydrogenation catalyst and applications thereof |
| US10335773B2 (en) | 2013-07-18 | 2019-07-02 | China University of Petroleum—Beijing | Fe-based hydrogenation catalyst and use thereof |
| CN104646006A (en) * | 2013-11-22 | 2015-05-27 | 中国石油天然气股份有限公司 | Load type hydrodenitrogeneration catalyst and preparation method thereof |
| CN104646006B (en) * | 2013-11-22 | 2017-04-05 | 中国石油天然气股份有限公司 | A kind of load hydrogenation denitrification catalyst and preparation method thereof |
| CN104826584A (en) * | 2015-04-22 | 2015-08-12 | 芜湖市鸿坤汽车零部件有限公司 | Multi-plant modified composite active carbon particle with devulcanization effect and preparation method thereof |
| CN106925285A (en) * | 2015-12-29 | 2017-07-07 | 中国石油天然气股份有限公司 | Heavy-oil hydrogenation catalyst and preparation method thereof |
| CN106925285B (en) * | 2015-12-29 | 2019-12-06 | 中国石油天然气股份有限公司 | Heavy oil hydrogenation catalyst and preparation method thereof |
| CN108404897A (en) * | 2017-02-10 | 2018-08-17 | 中国石油天然气股份有限公司 | A kind of catalyst carrier for hydrgenating heavy oil, preparation method, using its catalyst and catalyst preparation method |
| CN108144626A (en) * | 2017-11-27 | 2018-06-12 | 南京工业大学 | A kind of lamellar composite type Hydrobon catalyst and preparation method |
| CN108144626B (en) * | 2017-11-27 | 2021-02-19 | 南京工业大学 | Layered composite hydrodesulfurization catalyst and preparation method thereof |
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Application publication date: 20110504 |