CN103785397B - A kind of removal of ccr by hydrotreating Catalysts and its preparation method - Google Patents
A kind of removal of ccr by hydrotreating Catalysts and its preparation method Download PDFInfo
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- CN103785397B CN103785397B CN201210427641.6A CN201210427641A CN103785397B CN 103785397 B CN103785397 B CN 103785397B CN 201210427641 A CN201210427641 A CN 201210427641A CN 103785397 B CN103785397 B CN 103785397B
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Abstract
The present invention discloses a kind of removal of ccr by hydrotreating Catalysts and its preparation method.This catalyst take aluminium oxide as carrier, and with Mo, Ni for active component, content meter by weight, containing the MoO of 10% ~ 20% in catalyst
3, the NiO of 2% ~ 5%; The surface area of catalyst is 150 ~ 210m
2/ g; Pore volume is 0.5 ~ 0.90mL/g, and in pore size distribution, the hole of 6 ~ 10nm accounts for hole that total pore volume is no less than 50%, more than 100nm and accounts for total pore volume and be no less than 10%.A kind of preparation method of removal of ccr by hydrotreating catalyst, comprise the steps: to pass into alkaline precipitating agent after (1) acid aluminium salt aqueous solution and the alkali metal aluminate aqueous solution carry out neutralization reaction or the basic aluminate aqueous solution regulates slurry pH value to be 8.5-9.7, in 150-220 DEG C, lower aging 0.1-2 hour; (2) step (1) aging after material after filtration, washing, add 10 ~ 40wt% aluminium carbonate ammonium after drying and carry out shaping; (3) the material load active component after shaping, obtained removal of ccr by hydrotreating catalyst after drying, roasting.This catalyst there is higher demetalization and desulphurizing activated while to have high de-carbon residue active.
Description
Technical field
The present invention relates to a kind of removal of ccr by hydrotreating Catalysts and its preparation method, relate to a kind of high activity in particular, low cost residual hydrogenation takes off carbon residue Catalysts and its preparation method.
Background technology
In residual hydrocracking technique, the impurity content of raw material is higher, especially the metal impurities such as oil-soluble nickel and vanadium, and the inactivation for hydrodesulfurization, denitrification catalyst has important impact.Current many technology propose the method removing this type of impurity from charging, to protect downstream high activity desulphurization and denitrification catalyst.US447314 proposes a kind of grating of dual catalyst bed system hydrotreatment residual oil; this grating first loads macroporous catalyst; then small catalyst below; feedstock oil sequentially passes through beds; realize macroporous catalyst and remove metal impurities, protect the desulfurization removing nitric activity that small catalyst below keeps higher.US4306964 proposes three kinds of catalyst and loads successively, solves the problem.CN200310104914 proposes denitrification catalyst position and adopts anti-grading loading mode, and denitrification catalyst aperture, downstream is slightly larger than upstream denitrification catalyst, and activity is also a little less than upstream denitrification catalyst, to control bed temperature rise, and extension fixture running life.The feature of residual oil raw material is that molecule is large, and complex structure, saturation degree is low, and aromaticity is high, and impurity content is high.The predecessor of carbon residue is exactly the high large molecule aromatic hydrocarbons (comprising asphalitine and colloid) of aromaticity.Although protective agent and catalyst for demetalation can do and remove most of metal impurities, part carbon residue can only be removed, also have carbon residue predecessor to be greatly deposited on above desulphurization and denitrification catalyst below, cause desulphurization and denitrification catalyst inactivation.Above-mentioned patent all ignores the precipitation after hydrogenation on the armaticity macromolecular catalyst such as asphalitine and heavy colloid, how better can optimizing the deposition on the catalyst of carbon deposit, becoming another major issue except removing metal impurities.Can not improve the activity of protective agent and catalyst for demetalation at present, otherwise can cause a large amount of Impurity deposition, catalyst temperature rise is higher, thus occurs focus or higher pressure drop, causes device to be stopped work.
Thus; CN03133994 proposes the de-carbon residue catalyst of filling between desulphurization catalyst and denitrification catalyst; this decarburization catalyst have employed two kinds of catalyst and carries out Gradation Optimization; first large aperture catalyst is adopted; then small-bore catalyst is loaded; metal component content all adopts denitrification catalyst tenor, so that large molecule aromatic deposits herein thus protects denitrification catalyst below.This patent adopts large aperture catalyst, and this catalyst specific surface can only control at 150m
2/ below g, reduces the activity of catalyst desulfurizing and denitrogenation, and two kinds of catalyst pore volumes only have 0.4 ~ 0.55cm
3/ g, be unfavorable for a large amount of asphalitine and colloid deposition in the catalyst.Known in sum, prepare that a kind of to have higher de-carbon residue, demetalization and desulphurizing activated catalyst significant.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of removal of ccr by hydrotreating Catalysts and its preparation method.This catalyst there is higher demetalization and desulphurizing activated while to have high de-carbon residue active.
A kind of removal of ccr by hydrotreating catalyst take aluminium oxide as carrier, and with Mo, Ni for active component, content meter by weight, containing the MoO of 10% ~ 20% in catalyst
3, the NiO of 2% ~ 5%; The surface area of catalyst is 150 ~ 210m
2/ g, is preferably 160 ~ 190m
2/ g; Pore volume is 0.5 ~ 0.90mL/g, is preferably 0.6 ~ 0.80mL/g; In pore size distribution, the hole of 6 ~ 10nm accounts for total pore volume and is no less than 50%, and the hole being preferably 55% ~ 65%, more than 100nm accounts for total pore volume and is no less than 10%, is preferably 10% ~ 20%.
A preparation method for removal of ccr by hydrotreating catalyst, comprises the steps:
(1) alkaline precipitating agent is passed into after the acid aluminium salt aqueous solution and the alkali metal aluminate aqueous solution carry out neutralization reaction or the basic aluminate aqueous solution regulates slurry pH value to be 8.5-9.7, be preferably 9.0-9.6, in 150-220 DEG C, lower aging 0.1-2 hour, preferably aging 0.1-1 hour at 170-200 DEG C;
(2) step (1) aging after material after filtration, washing, add 10 ~ 40wt% aluminium carbonate ammonium (weighing scale by dried alumina dry glue) after drying and carry out shaping;
(3) the material load active component after shaping, obtained removal of ccr by hydrotreating catalyst after drying, roasting.
The acid aluminium salt aqueous solution described in the inventive method step (1) refers to AlCl
3, Al
2(SO
4)
3, Al (NO
3)
3, the suitableeest is Al
2(SO
4)
3, alkali metal aluminate refers to NaAlO
2or KAlO
2, alkaline precipitating agent refers to NaOH, (NH
4)
2cO
3, NH
4oH.The suitableeest is NH
4oH, (NH
4)
2cO
3.
Preferably add the aluminium carbonate ammonium of 15-30% in the inventive method step (2), filter, washing, dry, shapingly all adopt conventional method.
Described in the inventive method step (3), load active component is realized by infusion process, preferred co-impregnation.Co-impregnated solution is by the calculating composition preparation for Kaolinite Preparation of Catalyst, sprayed in the carrier strip prepared, spray step to ensure solution just loaded body all to absorb and without unnecessary, therefore need the water absorption measuring carrier before dipping, thus determine the concentration using solution.When with molybdenum and nickel for active component time, preparation co-impregnated solution can use industrial ammonium heptamolybdate or molybdenum oxide, industrial nitric acid nickel or basic nickel carbonate to be raw material, and co-impregnated solution compositional range is: MoO
38.0 ~ 19.0g/100mL, NiO2.0 ~ 4.5g/100mL.
Catalyst of the present invention adopts the alumina dry glue of high temperature and high ph-values burin-in process, and this dry glue degree of crystallinity is high, and amorphous alumina is few, and crystal grain is relatively large.The minimizing of amorphous alumina content, impels inter-particle voids to increase, and boehmite size of microcrystal is relatively uniform, impels concentrating of catalyst aperture.This alumina dry glue and the aluminium carbonate ammonium shaping rear obtained catalyst that is mixed has the pore size distribution of more than the 100nm of concentrated pore size distribution between 6 ~ 10nm and adaptation, and active component content is few, de-carbon residue, demetalization and desulphurizing activated height.
Detailed description of the invention
The effect of the inventive method is illustrated below in conjunction with embodiment and comparative example.But following examples are not construed as limiting the invention.
The concrete preparation process of catalyst of the present invention is as follows: (1) prepares the acid aluminium salt aqueous solution, Al
2o
3concentration is 2 ~ 10g/100mL; (2) the basic aluminate aqueous solution is prepared, Al
2o
3concentration is 8 ~ 30g/100mL, or preparation dilute ammonia solution, NH
3content is 8 ~ 16g/100mL; (3) the acid aluminium salt aqueous solution and the basic aluminate aqueous solution join in the certain water gaging under stirring simultaneously continuously, and neutral temperature is 50-80 DEG C, comparatively fits as 55-75 DEG C, and the suitableeest is 60-70 DEG C; In and pH be 6.0-8.5, comparatively suitable 6.5-8.0, the suitableeest is 7.0-8.0; In and time range be 0.25-3 hour, comparatively suitable 0.5-2 hour, the suitableeest be 0.8-1.5 hour, in slurries Al
2o
3content 5-10wt%; (4) alkaline precipitating agent or the basic aluminate aqueous solution regulate slurry pH value to be 8.5-9.7, are preferably 9.0-9.6, in 150-220 DEG C, and lower aging 0.1-2 hour, preferably aging 0.1-1 hour at 170-200 DEG C; (5) filter, wash, drying 2 ~ 10 hours at 50 ~ 140 DEG C of temperature, the alumina dry glue (6) of system adds 10 ~ 40wt% aluminium carbonate ammonium kneading in alumina dry glue, shaping, drying 2 ~ 10 hours at 50 ~ 140 DEG C of temperature, rise to 550 ~ 700 DEG C with 200 ~ 300 DEG C/h of warm speed, constant temperature carries out carrier calcination under condition in 2 ~ 5 hours; (7) adopt co-impregnation load active component Mo, Ni, at 50 ~ 140 DEG C of temperature, drying 2 ~ 10 hours, rises to 470 DEG C ~ 550 DEG C with 150 ~ 200 DEG C/h, the catalyst of constant temperature 1 ~ 6 hour system.
Example 1
By the 2L sodium metaaluminate aqueous solution (Al
2o
3concentration is 15g/100mL) and the aqueous solution (Al of 3L aluminum sulfate
2o
3concentration is 4g/100mL) be respectively charged in the container of high level, lower even flowmeter flows into and is equipped with in the belt stirrer of 6L water purification and the rustless steel container of heating jacket, is heated to 60 DEG C.Under agitation, two kinds of materials are added in stainless cylinder of steel by certain speed simultaneously, keep pH be 7.2, in and 1 hour, in and slurries Al
2o
3content 8wt%.After neutralization terminates, use NH
4oH adjusting slurry pH value is 9.6, in closed container, slurry temperature is risen to 180 DEG C, after aging 0.3 hour, and isolated by filtration place mother liquor, washing.At 140 DEG C of temperature after dry 3 hours, add 30% aluminium carbonate ammonium kneading and compacting, at 100 DEG C of temperature, after dry 5 hours, rise to 600 DEG C, constant temperature 4 hours obtained alumina supports with 200 DEG C/h of programming rates; Co-impregnation load active component, altogether MoO in maceration extract
315.0g/100mL, NiO3g/100mL, after spray dipping at 110 DEG C of temperature dry 5 hours, rise to 500 DEG C with 180 DEG C/h, constant temperature 3 hours obtained catalyst 1, catalyst composition and character were in table 1.
Example 2
Prepare alumina support according to method described in embodiment 1, be not both and use NH
4oH adjusting slurry pH value is 9.0, and aging temperature is 200 DEG C, adds 15% aluminium carbonate ammonium kneading and compacting, obtains catalyst 2, and catalyst composition and character are in table 1.
Example 3
Prepare alumina support according to method described in embodiment 1, be not both use (NH
4)
2cO
3adjusting slurry pH value is 9.4, and aging temperature is 170 DEG C, adds 25% aluminium carbonate ammonium kneading and compacting, obtains catalyst 3, and catalyst composition and character are in table 1.
Example 4
Prepare alumina support according to method described in embodiment 1, not being both aluminium carbonate ammonium addition is 20%, obtains catalyst 4, and catalyst composition and character are in table 1.
Example 5
Prepare alumina support according to method described in embodiment 1, not being both neutral temperature is 70 DEG C, and aging 0.5h, obtains catalyst 5, and catalyst composition and character are in table 1.
Example 6
Prepare alumina support according to method described in embodiment 1, not being both aging temperature is 190 DEG C, and aging 0.8h, obtains catalyst 6, and catalyst composition and character are in table 1.
Comparative example 1
Prepare alumina support according to method described in embodiment 1, be not both and use NH
4oH adjusting slurry pH value is 8.0, and aging temperature is 120 DEG C, does not shapingly add aluminium carbonate ammonium, obtains catalyst 7, and catalyst composition and character are in table 1.
The physico-chemical property of table 1 hydrogenation catalyst
| Example | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| MoO 3Content/wt% | 15.0 | 15.2 | 15.1 | 14.9 | 15.0 | 14.8 | 15.1 |
| NiO content/wt% | 3.0 | 2.9 | 3.2 | 2.8 | 3.2 | 3.0 | 3.03 |
| Specific surface/m 2·g -1 | 190 | 180 | 179 | 192 | 185 | 196 | 210 |
| Pore volume, mL/g | 0.68 | 0.70 | 0.74 | 0.72 | 0.76 | 0.65 | 0.40 |
| Pore size distribution/% | |||||||
| <6nm | 12 | 8 | 9 | 15 | 4 | 17 | 50.1 |
| 6-10nm | 62 | 64 | 60 | 64 | 59 | 60 | 40.2 |
| 10~100nm | 11 | 13 | 15 | 8 | 20 | 10 | 9.7 |
| >100nm | 15 | 14 | 18 | 11 | 17 | 13 | 0 |
Implement 7
400mL fixed bed hydrogenation experimental rig has carried out evaluation test to catalyst 1 ~ 7, and feedstock oil character, experimental condition are as table 2,3, and result of the test is as shown in table 4.
Table 2 feedstock oil character
| Feedstock oil character | The normal slag in the Middle East |
| Carbon residue, % | 12.1 |
| S，w% | 3.8 |
| Ni，ug/ g | 32.2 |
| V，ug/g | 98.5 |
Table 3 experimental condition
| Reaction temperature, DEG C | 385 |
| Reaction pressure, MPa | 15.7 |
| Volume space velocity, h -1 | 1.0 |
| Hydrogen-oil ratio, V/V | 758 |
Table 4 evaluation result
| Example | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| HDM,% | 94.2 | 93.9 | 94.5 | 92.1 | 95.0 | 93.2 | 88.9 |
| HDS,% | 90.5 | 90.2 | 89.6 | 91.2 | 88.5 | 91.0 | 90.2 |
| HDCCR.% | 68.8 | 68.5 | 69.2 | 67.5 | 69.0 | 67.2 | 58.1 |
As can be seen from Table 1, catalyst 6 ~ 10nm aperture of preparing according to this patent is more concentrated, and has part 100nm aperture.As can be seen from Table 4, the catalyst by removing metals prepared of this patent is active and de-carbon residue activity is higher.
Claims (9)
1. a removal of ccr by hydrotreating catalyst, take aluminium oxide as carrier, with Mo, Ni for active component, it is characterized in that: content meter by weight, containing the MoO of 10% ~ 20% in catalyst
3, the NiO of 2% ~ 5%; The surface area of catalyst is 150 ~ 210m
2/ g; Pore volume is 0.5 ~ 0.90mL/g; In pore size distribution, the hole of 6 ~ 10nm accounts for hole that total pore volume is no less than 50%, more than 100nm and accounts for total pore volume and be no less than 10%.
2. catalyst according to claim 1, is characterized in that: the surface area of catalyst is 160 ~ 190m
2/ g; Pore volume is 0.6 ~ 0.80mL/g; In pore size distribution the hole of 6 ~ 10nm account for total pore volume be 55% ~ 65%, more than 100nm to account for total pore volume be 10% ~ 20% in hole.
3. the preparation method of catalyst described in claim 1, is characterized in that: comprise the steps:
(1) alkaline precipitating agent is passed into after the acid aluminium salt aqueous solution and the alkali metal aluminate aqueous solution carry out neutralization reaction or the basic aluminate aqueous solution regulates slurry pH value to be 8.5-9.7, aging 0.1-2 hour at 150-220 DEG C;
(2) step (1) aging after material after filtration, washing, add 10 ~ 40wt% after drying and undertaken shaping by the aluminium carbonate ammonium of dried alumina dry glue weighing scale;
(3) the material load active component after shaping, obtained removal of ccr by hydrotreating catalyst after drying, roasting.
4. method according to claim 3, is characterized in that: adjustment slurry pH value is 9.0-9.6, aging 0.1-1 hour at 170-200 DEG C.
5. method according to claim 3, is characterized in that: the acid aluminium salt aqueous solution described in step (1) refers to AlCl
3, Al
2(SO
4)
3, Al (NO
3)
3, alkali metal aluminate refers to NaAlO
2or KAlO
2, alkaline precipitating agent refers to NaOH, (NH
4)
2cO
3, NH
4oH.
6. method according to claim 3, is characterized in that: the acid aluminium salt described in step (1) is Al
2(SO
4)
3, alkaline precipitating agent is NH
4oH, (NH
4)
2cO
3.
7. method according to claim 3, is characterized in that: the aluminium carbonate ammonium adding 15-30% in step (2).
8. method according to claim 3, is characterized in that: described in step (3), load active component is realized by infusion process.
9. the method according to claim 3 or 8, is characterized in that: load active component described in step (3) adopts co-impregnation, and co-impregnated solution compositional range is: MoO
38.0 ~ 19.0g/100mL, NiO2.0 ~ 4.5g/100mL.
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