CN105709806B - Dispersed hydrocracking catalyst of a kind of group VIII metal and preparation method thereof - Google Patents
Dispersed hydrocracking catalyst of a kind of group VIII metal and preparation method thereof Download PDFInfo
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Abstract
The present invention, which discloses a kind of hydrocracking catalyst preparation process, includes following content：（1）Prepare carrier of hydrocracking catalyst；（2）The metal salt solution containing hydrogenation active component is prepared, hydrogenation active component is generally W, Mo of group vib and the Ni of VIII and Co is applied in combination, by step（1）The catalyst carrier of middle preparation carries out supersaturated dipping, then filters redundant solution；（3）By step（2）The wet bar of catalyst of preparation is placed in impregnation in the organic solution of ammonia, then separation of solid and liquid, and finished catalyst is obtained through drying, roasting.Catalyst group VIII metal prepared by this method is uniformly dispersed.
Description
Technical field
The present invention relates to dispersed hydrocracking catalyst of a kind of group VIII metal and preparation method thereof.
Background technology
As crude quality becomes weight, variation year by year, environmental regulation is increasingly strict, and market is continuous to the demand of clear gusoline
Increase so that the hydrogen addition technology for producing clean fuel obtains more and more extensive application.In the secondary operation technology of crude oil, evaporate
Point oily hydrocracking technology has the characteristics that strong adaptability to raw material, production operation and products scheme flexibility is big, good product quality,
Various heavys, inferior raw material can be converted into the high-quality jet fuel of market in urgent need, diesel oil, lube basestocks and
Chemical industry naphtha and tail oil preparing ethylene by steam cracking raw material etc., play product distribution in full factory's production procedure and product quality is adjusted
The effect of device is saved, is the core that " oil-change-fibre " combines, it has also become most important heavy oil in modern times oil refining and petro chemical industry
One of deep processing technique.From nineteen fifty-nine Chevron company Isocracking hydrocracking technology first in California, USA Ritchie
Since covering oil plant commercial Application, the development and application of hydrocracking technology obtains swift and violent development.CLG companies, UOP are public
External major refining such as department, Criterion catalyst Co.s, Albemarle companies, Haldor Topsoe companies and Axens companies
Oily company and R＆D institution increase the input of technological innovation, and significant progress is obtained in terms of hydrocracking technology exploitation.Cut
Only 2012, the global total working ability of hydrocracking unit reached more than 2.78Mt/a, accounts for crude oil time processing ability
6.26%。
China is one of country for grasping distillate hydrocracking technology earliest in the world, is early in last century the fifties
Distillate hydrocracking technology is started to develop, and is voluntarily set using the complete set technology of oneself domestic exploitation in the sixties in last century
Count China's first set distillate hydrocracking device that has been constructed and put into operation.Into 21 century, with rapid development of economy, oil production
The demand rapid growth of product, CNPC's consumption reaches 4.67 hundred million tons within 2012, occupies second place of the world.At the same time, China
It is hydrocracked working ability and also obtains swift and violent development, throughput has reached 60.0Mt/a, accounts for crude oil time processing energy
Nearly the 12% of power, far above world average level.But hydrocracking technology application market development in China's is weighed with skewness, place
Reason ability is concentrated mainly on state-owned large-scale oil refining enterprise, and the technological process of use is more single, and most tail oil products are as ethene
Cracking stock.As crude oil in China quality becomes weight, variation year by year, the processing capacity of sour crude increases year by year, and environmental protection is to refining oil work
Skill is in itself and petroleum product-quality requires increasingly strict, lasting increasing of the market to clean fuel oil and high-quality chemical industry raw materials requirement amount
Long, hydrocracking technology will be also more widely applied at home, and market competition will be growing more intense, while also hydrogenation is split
Change technical merit and propose higher requirement.
The core of hydrocracking technology is hydrocracking catalyst, and the technology of its technology depends on carrying for catalyst performance
Rise.Hydrocracking catalyst is bifunctional catalyst, comprising adding dehydrogenation functionality and cracking function.Usual cracking function is carried by acidity
Body component provides, and mainly includes molecular sieve and amorphous oxide.And add dehydrogenation functionality mainly to be provided by hydrogenation metal, hydrogenation gold
Category generally comprises conventional non-noble metal components, such as W, Mo, Ni, Co, and noble metal is typically chosen Pt, Pa.It is hydrocracked and urges
Incorporation way generally use kneading method, beating method, coprecipitation method and infusion process of non-noble metal components etc. in agent, wherein with dipping
Method is the most commonly used, accounts for existing commercial Application hydrocracking catalyst more than 80%.Infusion process prepares hydrocracking catalyst, system
Standby range request hydrogenation metal salt of crossing can make the metal salt solution that stability is good, concentration is high.Hydrocracking catalyst category
In fine chemical product, preparation technology is complicated, and production process is restricted by many factors.The hydrogenation activity of hydrocracking catalyst
The metal component in VI B races in the periodic table of elements and VIII race, most widely used is in tetra- kinds of metals of W, Mo, Ni, Co
It is one or more of.Wherein metallic nickel（Or metallic cobalt）It is the most frequently used metal promoter component of hydrocracking catalyst.In order to ensure
The materialization of hydrocracking catalyst and catalytic performance, the metallic salt for requiring to introduce in its preparation process remove after Roasting Decomposition
Outside oxygen element, remained without other elements.When preparing hydrocracking catalyst using infusion process and coprecipitation method, it is also necessary to configure
The metal salt solution that concentration is high, stability is good.Nickel metal（Or cobalt）Salt in, nitrate has that solubility is high, solution is steady
After qualitative good, decomposition the advantages that noresidue, it is widely used in hydrocracking catalyst preparation process.Patent
CN96109702.7 provides a kind of co-impregnated solution for preparing high-activity hydrocracking catalyst, is helped by ammonium metatungstate, nickel nitrate one kind
Preserved material, obtained with carrier prepared catalyst performance of the co-impregnated solution dipping containing Y type molecular sieve, refractory inorganic oxides bright
Aobvious lifting.Patent CN88103069.4 gives a kind of preparation method of supported non-noble metal hydrocracking catalyst, its
Active component is VI B races and/or VIII B races non-noble metal j element in the periodic table of elements, and metal incorporation way is mainly using leaching
Stain method.Middle distillate selectivity of product keeps gas in constant, product to generate when the catalyst of preparation has reaction temperature rise
Amount less, coking situation be similar to using conventional molecular sieve as acidic components catalyst the characteristics of, suitable for mild hydrocracking.Patent
US5,229,347 give a kind of preparation method of hydrocracking catalyst, and this prepares catalyst and includes VIB and VIII groups
Metal component is closed, after catalyst carrier shaping, metal component is introduced using infusion process, dipping rear catalyst is by drying, roasting
The step of burning, prepares finished catalyst.
Hydrocracking catalyst prepared by the above method, easily causes hydrogenation metal, such as group VIII metal component, concentrates
Into carrier surface microcellular structure, particularly in the microcellular structure of molecular sieve component, cause metal dispersion uneven, due to reaction
Thing hydrocarbon component is difficult to enter in the less microcellular structure of diameter, also reduces these utilizations for entering microcellular structure metal
Rate.
The content of the invention
In view of the shortcomings of the prior art, the present invention provide a kind of dispersed hydrocracking catalyst of group VIII metal and
Its preparation method.
Hydrocracking catalyst preparation process of the present invention includes following content：
（1）Selective hydrocracking catalyst carrier material powder, carrier material include at least one acid cracking material, added
Enter Aci-Jel solvent or binding agent, by kneading, roll, extrusion, pelletizing, drying and roasting, prepare hydrocracking catalyst
Carrier；
（2）The metal salt solution containing hydrogenation active component is prepared, hydrogenation active component is generally W, Mo and VIII of group vib
The Ni and Co of race are applied in combination, by step（1）The catalyst carrier of middle preparation carries out supersaturated dipping, then filters unnecessary molten
Liquid；
（3）By step（2）The wet bar of catalyst of preparation is placed in impregnation in the organic solution of ammonia, then separation of solid and liquid,
Finished catalyst is obtained through drying, roasting.
Step of the present invention（1）Described in acid cracking material include molecular sieve or amorphous acidic components, molecular sieve one
As include one kind or several in Y type molecular sieve, beta-molecular sieve, ZSM-5 molecular sieve, SAPO molecular sieve, MCM-41 mesopore molecular sieves etc.
Kind, amorphous acidic components are generally the one or more in amorphous silica-alumina, amorphous silicon magnesium, clay etc..Required molecule
Sieve can require to carry out suitable modification according to performance.In hydrocracking catalyst carrier material can also include it is acid compared with
Weak inorganic refractory oxide, generally aluminum oxide or aluminum oxide containing auxiliary agent, during use typically using aluminum hydroxide solid elastomer powder as
Raw material.There is big pore volume, the raw material of bigger serface in the preferably this area such as amorphous acidic components and aluminum oxide.
Step of the present invention（1）Middle peptizing agent is generally acid solution, such as dust technology, and binding agent is generally by peptization
Small porous aluminum oxide；Banded extruder orifice plate can be cylinder, clover, bunge bedstraw herb or other irregular shape catalysts.
Step of the present invention（2）In the metal salt solution containing hydrogenation active component in, it is suitable to be added as needed on
Contain one or more of compounds in P, F, B, Zr, Ti in adjuvant component, such as dipping solution.
Step of the present invention（3）Ammonia mass concentration is 0.5% ~ 30% in the organic solution of middle ammonia, and solvent can be with organic solution
It is the one or more in methanol, ethanol, ethylene glycol, ether, impregnates solid-to-liquid ratio 1:1~1:10,30 ~ 180min of processing time, place
Manage 20 ~ 80 DEG C of temperature.
Step of the present invention（3）Middle 40 ~ 90 DEG C, 1 ~ 4h of time of drying temperature, 300 ~ 700 DEG C of sintering temperature, roasting time 3 ~
12h。
Hydrocracking catalyst prepared by the above method, based on weight content in final catalyst, acidic support material one
As content be 1% ~ 70%, weight content of the hydrogenation active component in terms of oxide in the catalyst is generally 15% ~ 50%, be preferably
20% ~ 40%, while can be with salic less than 50%, specific surface area of catalyst 150m2/g~450m2/ g, preferably 220m2/
g~400m2/g；Pore volume is 0.2cm3/g~0.7cm3/ g, preferably 0.3cm3/g~0.6cm3/g；5 ~ 20nm of average pore size, preferably 7 ~
15nm；VIII metal oxide contents are 2.0% ~ 15.0%；0.60 ~ 1.20g/mL of bulk density.
The inventive method suitable quantity of water, ammonia and is had using the catalyst wet bar of the organic solution processing supported active metals of ammonia
The system of solvent composition, can effectively prevent the accumulation of metal caused by drying with the capillarity in roasting process
Problem so that VIII metals are uniformly distributed, and greatly improve the utilization ratio of VIII group metals, hence it is evident that improve catalyst hydrogenation
Energy.Compared with only being played a role with routine to the group VIII metal on top layer using ammonia spirit or ammonia gas phase treatment,
This method can cause the uniform Precipitation of group VIII metal in catalyst, rather than ammonia gas phase treatment method due to liquid
Surface tension effects.
The inventive method can be such that VIII metals are evenly distributed on the surface area of macropore, improve the utilization of metal
Rate, when preparing Hydrogenation identical hydrocracking catalyst, the less VIII metal components of content can be used, reduction is urged
The preparation cost of agent, at the same also cause catalyst pore structure obtain it is further improve, improve catalyst anti-coking and
Carbon distribution performance.
The inventive method is applicable not only to the preparation of the Cracking catalyst of load hydrogenation containing VIII, is further widely applied to other
The refined preparation with hydrotreating catalyst of load hydrogenation containing VIII, the hydrogenation saturation performance for improving hydrogenation catalyst
Improved significantly with hydrogenation abjection impurity performance.
In the preparation process of hydrocracking catalyst of the present invention, after the organic solvent processing of ammonia, organic solution can reclaim
Use, energy consumption, material consumption are low, and processing procedure is simple, and running cost is low, and suitable commercial scale is promoted the use of.The catalyst of preparation by
In with higher hydrogenation activity, suitable for the hydrocracking reaction process of more heavy, inferior raw material.
Brief description of the drawings
Fig. 1 is the group VIII metal distribution map of catalyst prepared by embodiment 1, embodiment 4, comparative example 1 and comparative example 2.
Test process is as follows：Embodiment HC-1, HC-4 catalyst and HC-B1, HC-B2 comparative example catalyst are vulcanized, to vulcanization
Catalyst afterwards has carried out power spectrum elementary analysis, and accompanying drawing gives the distribution of metal of the cylindrical catalyst from the center of circle to circumference.
The group VIII metal of embodiment catalyst is not changed significantly from the center of circle to circumference, is distributed than more uniform, and Reference Example is catalyzed
The group VIII metal distribution of agent is relatively uneven.
Embodiment
A kind of concrete processing procedure of hydrocracking catalyst of the present invention is as follows：
（1）Selective hydrocracking catalyst carrier material powder, carrier material include at least one acid cracking material, especially
It is the modified molecular screen catalysis material containing a large amount of microcellular structures；Add Aci-Jel solvent or the binding agent such as nitric acid, by kneading,
Roll, extrusion, pelletizing, drying and roasting, prepare carrier of hydrocracking catalyst；Catalyst shape is decided by banded extruder orifice plate
Pattern, can be cylinder, clover, bunge bedstraw herb or other irregular shape catalysts.
（2）The metal salt solution containing hydrogenation active component is prepared, hydrogenation active component is generally W, Mo and VIII of group vib
The Ni and Co of race are applied in combination, by step（1）The catalyst carrier of middle preparation carries out supersaturated dipping, dip operation solid-to-liquid ratio 1:
1~1:6, then filter redundant solution；
（3）The wet bar of rear catalyst will be impregnated to be placed in the organic solution of ammonia, the operation impregnated, solid-to-liquid ratio 1:1~1:
10, ammonia density 0.5% ~ 30%, 30 ~ 180min of processing time, 20 ~ 80 DEG C for the treatment of temperature, then separation of solid and liquid, low temperature drying removes
Unnecessary organic solvent, then carry out calcination activation and obtain finished catalyst, 40 ~ 90 DEG C, 1 ~ 4h of time of drying temperature, sintering temperature
300 ~ 700 DEG C, 3 ~ 12h of roasting time.
The following examples are used to processing method of the present invention be described in more detail, but the scope of the present invention is not limited solely to these
The scope of embodiment.
The aluminum hydroxide solid elastomer powder used in embodiment is that Tianjin Tian Jiu companies produce 3824 macroporous aluminium oxides, 400 DEG C of roastings
Property is pore volume 0.82mL/g, specific surface area 323m after burning 3 hours2/g。
The contained amorphous silica-alumina dry glue powder used in embodiment be Tianjin Tian Jiu companies produce 3903 amorphous silica-aluminas, 400 DEG C
Property is pore volume 0.76mL/g, specific surface area 286m after being calcined 3 hours2/ g, meleic acid 0.744mmol/g.
Embodiment 1
Contain Y molecular sieve 30% based on final hydrocracking catalyst weight, containing amorphous silica-alumina 15%, containing nickel oxide 5.0%,
Containing tungsten oxide 22.0%, surplus is that aluminum oxide selects Above-mentioned catalytic agent preparing raw material：HY molecular sieves, 3824 aluminum hydroxide solid elastomer powder
With 3903 contained amorphous silica-alumina dry glue powder.
Catalyst preparation process is as follows：HY molecular sieves hydro-thermal process at 550 DEG C, pressure 0.2MPa, time 90min.Take
Molecular sieve 98g is placed in stir process in 270mL dilute nitric acid solutions, 65 DEG C of temperature, time 40min after hydro-thermal process；Molecule screening the pulp
Liquid solid-liquid does not separate, and is directly mixed with aluminum hydroxide solid elastomer powder and contained amorphous silica-alumina dry glue powder, adds sesbania powder, expanding agent etc.
Component, extruded moulding is rolled, be extruded into a diameter of 1.5mm cylindrical types.Through 120 DEG C of dry 3h, 550 DEG C of roasting 3h.Then using steaming
Distilled water makes the mixed solution of ammonium metatungstate and nickel nitrate, and it is 1 that preformed catalyst carrier is carried out into solid-to-liquid ratio:2 supersaturation
Dipping, time 2h, filters redundant solution；The catalyst of impregnating metal solution is placed in the ethanol solution of ammonia, solid-to-liquid ratio 1:2,
Ammonia mass concentration 5.0%, processing time 60min, 35 DEG C for the treatment of temperature, then separation of solid and liquid, 60 DEG C of dryings, time 2h；Then enter
Row roasting, 500 DEG C of temperature, roasting time 6h, prepares finished catalyst.Catalyst numbering is respectively HC-1.
Embodiment 2
Metal salt solution in example 1 is changed to Mo-Ni-P solution, the organic solvent of ammonia replaces with methanol, and mass concentration is
12%, for other preparation methods with embodiment 1, it is HC-2 to obtain catalyst numbering.
Embodiment 3
Nickel nitrate in example 1 is changed to cobalt nitrate, for other preparation methods with embodiment 1, it is HC- to obtain catalyst numbering
3。
Embodiment 4
Contain nickel oxide 3.0% based on final hydrocracking catalyst weight, containing tungsten oxide 22.0%.The same embodiment of preparation method
1, it is HC-4 to obtain catalyst numbering.
Comparative example 1
Organic ammonia solution processing procedure in example 1 is changed to, the processing of 1.0Mpa ammonias, time 60min, 260 DEG C of temperature,
For other preparation process with example 1, it is HC-B1 to obtain catalyst numbering.
Comparative example 2
Organic ammonia solution in example 1 is handled, is changed to AMMONIA TREATMENT, ammonia concn 5%, other preparation process are the same as real
Example 1, it is HC-B2 to obtain catalyst numbering.
In the present embodiment, each example catalyst carries out instrumental analysis and activity rating to more than.Each example catalyst physico-chemical property
It is shown in Table 1.
The catalyst physico-chemical property of table 1.
Note：RBETFor the average pore diameter of BET method measure.
Evaluating apparatus uses to be carried out on 200mL small hydrogenation devices, and presulfurization is carried out to catalyst before activity rating.Evaluation
The raw materials used oil nature of catalyst activity is shown in Table 2, and catalyst reaction performance comparison the results are shown in Table 3.Evaluate HC-1, HC-4 and HC-
B1 has carried out comparative evaluation, and feedstock oil first passes through Hydrobon catalyst bed and then immediately proceeds to hydrocracking catalyst bed
Layer, by controlling the organic nitrogen content in feedstock oil to be less than 10ug/g during Hydrobon catalyst bed.
The raw material oil nature of table 2.
The catalyst reaction performance comparison evaluation result of table 3.
Claims (9)
1. a kind of hydrocracking catalyst preparation process, it is characterised in that including following content：
（1）Selective hydrocracking catalyst carrier material powder, carrier material include at least one acid cracking material, add acid
Property peptizing agent or binding agent, by kneading, roll, extrusion, pelletizing, drying and roasting, prepare carrier of hydrocracking catalyst；
（2）Prepare the metal salt solution containing hydrogenation active component, hydrogenation active component for group vib W, Mo and VIII Ni and
Co is applied in combination, by step（1）The catalyst carrier of middle preparation carries out supersaturated dipping, then filters redundant solution；
（3）By step（2）The wet bar of catalyst of preparation is placed in impregnation in the organic solution of ammonia, then separation of solid and liquid, through dry
Dry, roasting obtains finished catalyst；
Wherein, step（3）Ammonia mass concentration is 0.5% ~ 30% in the organic solution of middle ammonia, and solvent is methanol, second in organic solution
One or more in alcohol, ethylene glycol, ether, impregnate solid-to-liquid ratio 1:1~1:10,30 ~ 180min of processing time, treatment temperature 20 ~
80℃。
2. preparation process according to claim 1, it is characterised in that：Step（1）Described in acid cracking material include
Molecular sieve or amorphous acidic components.
3. preparation process according to claim 2, it is characterised in that：Molecular sieve includes Y type molecular sieve, beta-molecular sieve, ZSM-
One or more in 5 molecular sieves, SAPO molecular sieve, MCM-41 molecular sieves, amorphous acidic components include amorphous silica-alumina, nothing
One or more in setting silicon magnesium, clay.
4. preparation process according to claim 1, it is characterised in that：Step（1）Carrier of hydrocracking catalyst material bag
Acid weaker inorganic refractory oxide is included, is aluminum oxide or aluminum oxide containing auxiliary agent.
5. preparation process according to claim 1, it is characterised in that：Step（1）Middle peptizing agent is acid solution；Binding agent
For by the small porous aluminum oxide of peptization；Banded extruder orifice plate is cylinder, clover or bunge bedstraw herb.
6. preparation process according to claim 1, it is characterised in that：Step（2）In the metal containing hydrogenation active component
In salting liquid, suitable adjuvant component is added as needed on, adjuvant component includes the one or more in P, F, B, Zr, Ti.
7. preparation process according to claim 1, it is characterised in that：Step（3）Middle 40 ~ 90 DEG C of drying temperature, the time 1 ~
4h, 300 ~ 700 DEG C of sintering temperature, 3 ~ 12h of roasting time.
A kind of 8. catalyst prepared using any preparation process of claim 1-7, it is characterised in that：By in final catalyst
Weight content meter, acidic support material content are 1% ~ 70%, and weight of the hydrogenation active component in terms of oxide in the catalyst contains
Measure as 15% ~ 50%, salic less than 50%, specific surface area of catalyst 150m2/g ~450m2/g；Pore volume is 0.2cm3/g~
0.7cm3/g；5 ~ 20nm of average pore size；VIII metal oxide contents are 2.0% ~ 15.0%；0.60 ~ 1.20g/mL of bulk density.
9. catalyst described in claim 8, it is characterised in that：Based on weight content in final catalyst, hydrogenation active component with
The weight content of oxide meter in the catalyst is 20% ~ 40%, specific surface area of catalyst 220m2/g~400m2/g；Pore volume is
0.3cm3/g~0.6cm3/g；7 ~ 15nm of average pore size.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103785448A (en) * | 2012-11-03 | 2014-05-14 | 中国石油化工股份有限公司 | A clean preparation method of a hydrogenation catalyst |
| CN103785447A (en) * | 2012-11-03 | 2014-05-14 | 中国石油化工股份有限公司 | A clean preparation method of a hydrocracking catalyst |
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| WO2013067323A1 (en) * | 2011-11-04 | 2013-05-10 | Saudi Arabian Oil Company | Hydrotreating and aromatic saturation process with integral intermediate hydrogen separation and purification |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103785448A (en) * | 2012-11-03 | 2014-05-14 | 中国石油化工股份有限公司 | A clean preparation method of a hydrogenation catalyst |
| CN103785447A (en) * | 2012-11-03 | 2014-05-14 | 中国石油化工股份有限公司 | A clean preparation method of a hydrocracking catalyst |
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