CN105618155B - Hydrogenation catalyst carrier and its application and hydrogenation catalyst and its application - Google Patents
Hydrogenation catalyst carrier and its application and hydrogenation catalyst and its application Download PDFInfo
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Abstract
The present invention provides a kind of hydrogenation catalyst carrier and its application, which includes：Composite molecular screen and heat-resistant inorganic oxide, wherein molecular sieve and two dimension that the composite molecular screen contains one-dimensional non-crossing pore passage structure intersect the molecular sieve of pore passage structure.The present invention provides a kind of hydrogenation catalyst and its application, which includes：Carrier and tool precious metal element with hydrogenation efficiency, the carrier are carrier of the present invention.Catalyst cracking performance containing aforementioned bearer of the present invention is low while having good stereoselectivity, long-chain normal paraffin can be effectively isomerized to the isoparaffin of unilateral chain, the yield of low pour point lubricating oil product oil can be dramatically increased using this catalyst in lube oil hydrogenation dewaxing technique.
Description
Technical field
The present invention relates to a kind of hydrogenation catalyst carrier and its application and a kind of hydrogenation catalyst and its applications.
Background technology
The isomerization reaction of n-alkane is the important reaction in petroleum refining process.The isomery of n-alkane in distillate
Change, the octane number of gasoline can be improved and improves the low temperature fluidity containing wax product.For diesel oil distillate and lube cut
In long-chain normal paraffin, industrially often using dewaxing method be separated.Dewaxing technique includes solvent dewaxing, urges
Change dewaxing and isomerization dewaxing.
Isomerization dewaxing is to keep the long-chain normal paraffin in wax component different using the bifunctional catalyst with special pore structure
Structure turns to the isoparaffin of unilateral chain and adds hydrogen open loop to be the monocyclic naphthenes of belt length side chain polycyclic ring alkane, and reaction product is still
It is so ideal lubricating oil component.Therefore, isomerization dewaxing has very high yield, is production high viscosity index (HVI), low condensation point, low waves
The ideal scheme of the top-grade lubricating oil of hair degree, has broad application prospects.
For gasoline component, isomerization of paraffins degree is higher, is more conducive to the octane number for improving gasoline.However it is right
For lubricating oil component, excessively high collateralization degree can be substantially reduced lubricating oil viscosity index, so to the different of lubricating oil
The selective isomerization performance that structure dewaxing catalyst requires, is embodied in：1. cracking performance is low, isomerization performance is high；2. unilateral
Long-chain normal paraffin can be selectively isomerized to the alkane of the unilateral chain of same carbon number by the high selectivity of chain hydrocarbon products.
Isomerization dewaxing catalyst is a kind of bifunctional catalyst, including acid function and hydrogenation/dehydrogenation function.Acid carrier
The acidic site of isomerization/cracking is provided, metal position provides hydrogenation/dehydrogenation function.Typically acid carrier includes mainly：It is amorphous
Oxide or oxide mixture, aluminosilicate-type molecular sieve, such as modenite, ZSM-5, ZSM-22；Silicoaluminophosphate molecular sieve analog,
Such as SAPO-11, SAPO-31, SAPO-41.Metal include precious metals pt, Pd or metal sulfide system (such as Ni/Co, Ni/W,
Ni/Mo sulfides), the latter contains sulfur feedstock for high.
The acidity (distribution of acid intensity and acidic site) of carrier and the balance of metallicity are to determine isomerization product choosing
The primary factor of selecting property.To heavier base oil fractions, only leans on and isomerization of paraffins is difficult to meet base oil strict demand
Cryogenic property.In recent years the study found that the catalysis combined with noble metal using the molecular sieve of the one-dimensional pore structure of middle strong acidity
The lube cut or soft wax of high-content wax are processed in agent, can produce the high-performance base oil of superhigh viscosity index.This is mainly
Since the catalyst has the very high isoparaffin selectivity by normal alkane isomerization for the unilateral chain with carbon number.
Chevron companies take the lead in having developed Isodewaxing isomerization dewaxing techniques using this kind of catalysis material.
When carrying out isomerization reaction, molecular sieving effect is presented as reactant selectivity or selectivity of product.It is former for mixing
All kinds of molecules in material, only can enter carrier duct and contact with the activated centre in duct, participate in react molecule could make
For reactant, and the molecule more than molecular sieve bore diameter will be excluded from except duct, be not involved in reaction, shown by this is exactly anti-
Answer the selectivity of object.And the bigger molecule or equilibrium conversion formed in duct is compared with small molecule effusion, or plugging hole on the spot
Road finally results in catalyst inactivation, and shown by this is exactly the selectivity of product.
It in shape selective catalysis, is not only due to molecule and penetrates molecular sieve aperture to be restricted and generate shape-selective effect, Er Qie
After molecule enters endoporus, the limitation of mass transfer is also suffered from.Especially when reactant or product molecule diameter and molecular sieve aperture are straight
When diameter is close, due to by inner hole wall field effect and various energy barriers hinder, molecule will be by various in transgranular diffusion
Limitation.The minor change of molecular sieve bore diameter or diffusing molecules diameter can all lead to the significant changes of diffusion coefficient.This variation is returned
Tie the variation of configuration when molecule penetrates molecular sieve aperture.At this point, diffusion is not only related with the length of molecule, but also and molecule
Internal motion is related.One is reacted by what configuration diffusion was limited, and reaction rate will be by catalyst grain size and active
It influences.
The selectivity of transition state.When reactant and product molecule can be spread in duct, but generate needed for final product
Transition state (reaction intermediates) it is big when, since the size or orientation of reaction intermediates need larger space, and molecular sieve pores
The useful space in road but very little, can not provide required space, then cannot form transition state in molecular sieve pore passage, at this time instead
It should can not carry out, to which reaction shows as transition state selectivity.This selectivity and mass transfer selectivity are different, it and molecule
Size or the activity for sieving crystal are unrelated, and are solely dependent upon aperture and the structure of molecular sieve.
It includes different type alkane, cycloalkane and virtue to be by the feedstock oil that hydroisomerizing dewaxing technique process is processed
The complex mixture of hydrocarbon, different types of reactant needs Different Pore Structures and acid molecular sieve, to improve target product
Yield reduces the generation of side reaction.
Invention content
The object of the present invention is to provide a kind of hydrogenation catalyst carrier and its application and a kind of hydrogenation catalyst and its
Using the hydrogenation catalyst containing the carrier is used to not only can effectively reduce when feedstock oil such as lube oil hydrogenation isomerization-visbreaking
Generate the pour point of oil, moreover it is possible to obviously increase the yield of high viscosity index (HVI) (VI) fluid product.
To realize foregoing purpose, according to the first aspect of the invention, the present invention provides a kind of hydrogenation catalyst carrier,
The carrier includes：Composite molecular screen and heat-resistant inorganic oxide, wherein the composite molecular screen contains one-dimensional non-crossing duct knot
The molecular sieve and two dimension of structure intersect the molecular sieve of pore passage structure.
According to the second aspect of the invention, the present invention provides a kind of hydrogenation catalyst, which includes：Carrier and tool
Precious metal element with hydrogenation efficiency, the carrier are carrier of the present invention.
According to the third aspect of the invention we, the present invention provides carrier and catalyst the answering in Hydrodewaxing of the present invention
With.
According to the fourth aspect of the invention, the present invention provides the carriers of the present invention and catalyst to add hydrogen in waxy feeds oil
Application in dewaxing.
Catalyst cracking performance containing aforementioned bearer of the present invention is low while having good stereoselectivity, can effectively by
Long-chain normal paraffin is isomerized to the isoparaffin of unilateral chain, can be shown using this catalyst in lube oil hydrogenation dewaxing technique
Write the yield for increasing low pour point lubricating oil product oil.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Fig. 1 is that the oily liquid in different pour points of generation that catalyst A, catalyst B, catalyst D1 and catalyst D2 are obtained is received
Figure.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
As previously mentioned, the present invention provides a kind of hydrogenation catalyst carrier, which includes：Composite molecular screen and heat-resisting
Inorganic oxide, wherein the molecular sieve and two dimension that the composite molecular screen contains one-dimensional non-crossing pore passage structure intersect duct knot
The molecular sieve of structure.
Support according to the present invention, preferably on the basis of the gross weight of carrier, the content of composite molecular screen is 20-90 weights
Measure %, preferably 50-60 weight %.
Support according to the present invention, molecular sieve and the two dimension of preferably one-dimensional non-crossing pore passage structure intersect point of pore passage structure
The weight ratio 3-12 of son sieve：1, preferably 6-9：1.
The aperture of support according to the present invention, the preferably described composite molecular screen is 5-20nm, pore volume 0.1-0.2ml/
g。
Support according to the present invention, the molecular sieve of the preferably described one-dimensional non-crossing pore passage structure be ZSM-22 molecular sieves,
It is one or more in SAPO-11 molecular sieves and SAPO-31 molecular sieves, more preferably ZSM-22 molecular sieves.
Support according to the present invention, preferably it is described two dimension intersect pore passage structure molecular sieve be beta-molecular sieve, modenite and
It is one or more in ZSM-5 molecular sieve, more preferably beta-molecular sieve.
According to a preferred embodiment of the present invention, the silica of ZSM-22 molecular sieves and the molar ratio of aluminium oxide are
71-73, the silica of beta-molecular sieve and the molar ratio of aluminium oxide are 29-30.
Support according to the present invention, the preferably described heat-resistant inorganic oxide are aluminium oxide, amorphous silicon aluminium, magnesia and oxygen
Change one or more in boron, preferably aluminium oxide and/or amorphous silicon aluminium.
As long as the purpose of the present invention can be realized in the carrier containing aforementioned component of the present invention, preparation method can be ability
The conventional selection in domain, the present invention can prepare this without particular/special requirement, such as the carrier of the present invention as follows：
By molecular sieve mixture (each molecular sieve component is added individually or together), heat-resistant inorganic oxide and/or heat-resisting
Inorganic oxide precursor body, extrusion aid, peptizing agent and water, which are mixed together, is rolled into plasticity object, is put into banded extruder extruded moulding
(shape according to being selected, for example, cylinder, cloverleaf pattern, butterfly etc.), then through drying, (such as temperature is 90-
150 DEG C) and roasting (such as temperature be 500-700 DEG C, time 2-6h) obtain carrier.
As previously mentioned, the present invention provides a kind of hydrogenation catalyst, which includes：Carrier and tool are with hydrogenation efficiency
Precious metal element, the carrier are carrier of the present invention.According to the present invention, the tool precious metal element with hydrogenation efficiency
Load is on the carrier.
Catalyst according to the invention, preferably on the basis of the gross weight of catalyst, it is total that the precious metal element accounts for catalyst
The 0.1-1 weight % of weight, more preferably 0.3-0.7 weight %.
Catalyst according to the invention, the one kind or more of the preferably described precious metal element in the VIIIth race's precious metal element
Kind, more preferably platinum and/or palladium.
Catalyst according to the invention, the precious metal element exist with oxidation state and/or reduction-state, it is however generally that, it is expensive
In the presence of metallic element is with oxidation state, catalyst is used to store and sell, and in the presence of precious metal element is with reduction-state, catalyst
For using, therefore precious metal element is typically prepared with hydrogenation catalyst existing for oxidation state, is stored and sold, and answering
With preceding, catalyst is restored, restoring method can be the conventional selection of this field, and reducing condition generally comprise：Hydrogen partial pressure
For 0.2-2MPa, 300-500 DEG C of temperature, time 1-10 hour.
As long as the purpose of the present invention can be realized in the catalyst containing aforementioned component of the present invention, preparation method can be this
The conventional selection in field, the present invention is to this without particular/special requirement, such as the catalyst of the present invention can be by preparing as follows：
(1) water-soluble precious metal salt (such as chloroplatinic acid, four ammonia platinum of dichloro and palladium nitrate) and deionized water are mixed into system
At aqueous solution, using saturation infusion process in supported on carriers hydrogenation activity noble metal；
(2) carrier containing hydrogenation activity noble metal is by 90-150 DEG C of dry and 350-550 DEG C of roasting 2-6h post-processing
Obtain catalyst.
The present invention provides the application of the carrier of the present invention and the catalyst of the present invention in Hydrodewaxing.
The present invention provides the application of the carrier of the present invention and the catalyst of the present invention in waxy feeds oil Hydrodewaxing.
In the present invention, the waxy feeds oil can be hydrocracking tail oil, atmospheric distillate, vacuum distillate and de- drip
Green decompression residuum.
Illustrate present disclosure below by embodiment, but it is not considered that present invention is limited only to embodiments below.
In the present invention, the aperture of composite molecular screen and pore volume are all made of BET method measurement.
In the present invention, in embodiment or comparative example, the molar ratio of the silica and aluminium oxide of the ZSM-22 molecular sieves used
Be 72, the silica of the beta-molecular sieve used and the molar ratio of aluminium oxide are 30, the silica of the SAPO-11 molecular sieves used with
The molar ratio of aluminium oxide is 0.4, the silica of the modenite used and the molar ratio 28 of aluminium oxide.
Embodiment 1
(aperture 5-20nm, pore volume are composite molecular screen by 100g simultaneously containing ZSM-22 molecular sieves and beta-molecular sieve
The weight ratio of 0.16ml/g, ZSM-22 molecular sieve and beta-molecular sieve is 6:1) with 100g alumina powders (production of South Africa SASOL companies)
Mixing, the aqueous solution of nitric acid that a concentration of 2 weight % is then added carry out kneading and are rolled into paste, by rolling, are sent into and squeeze
Machine is extruded into the cylindrical bars of diameter 1.6mm, then through 120 DEG C of dry 4h, and catalyst carrier A is obtained after 580 DEG C of roasting 4h；
With Pt (NH3)4Cl2Platinum is loaded to carrier by aqueous solution by being saturated dipping method, using 120 DEG C of dry 4h,
Catalyst A is obtained after 450 DEG C of roasting 4h, platinum content is 0.3 weight %.
Embodiment 2
Catalyst B is prepared according to the method for embodiment 1, the difference is that the weight ratio of ZSM-22 molecular sieves and beta-molecular sieve is
7:1, the dosage of composite molecular screen is 125g.
Embodiment 3
Catalyst C is prepared according to the method for embodiment 1, the difference is that the weight ratio of ZSM-22 molecular sieves and beta-molecular sieve is
9:1, the dosage of composite molecular screen is 150g.
Embodiment 4
Catalyst D is prepared according to the method for embodiment 1, the difference is that the weight ratio of ZSM-22 molecular sieves and beta-molecular sieve is
3:1。
Embodiment 5
Catalyst E is prepared according to the method for embodiment 1, the difference is that ZSM-22 molecular sieves are replaced by SAPO-11 molecular sieves,
Beta-molecular sieve is replaced by modenite.
Embodiment 6
According to catalyst F prepared by the method for embodiment 1, the difference is that the dosage of composite molecular screen is 233g.
Comparative example 1
Catalyst D1 is prepared according to the method for embodiment 1, the difference is that beta-molecular sieve is replaced by ZSM-22 molecular sieves, that is, is carried
Body contains only a kind of molecular sieve ZSM-22 molecular sieves.Remaining process is same as Example 1, obtains catalyst D1.
Comparative example 2
Catalyst D2 is prepared according to the method for embodiment 2, the difference is that ZSM-22 molecular sieves are replaced by beta-molecular sieve, that is, is carried
Body contains only a kind of molecular sieve beta-molecular sieve.Remaining process is same as Example 2, obtains catalyst D2.
Test case
Catalyst A, catalyst B, catalyst D1 and catalyst D2 are carried out in 20ml small fixed reactors respectively
(loaded catalyst 20ml, evaluation condition are shown in Table 1, and 2) raw material oil nature is shown in Table, evaluation result is shown in Table 3 for evaluation.
Wherein, catalyst prereduction, reducing condition are carried out before oil inlet first：Hydrogen partial pressure is 1.0MPa, and temperature is 450 DEG C,
Hydrogen flowing quantity is 10L/h, and the time is 8 hours.
Wherein, liquid of the generation oil that catalyst A, catalyst B, catalyst D1 and catalyst D2 are obtained in different pour points is received
See Fig. 1.
Table 1
| Project | Data |
| Reaction pressure/MPa | 12 |
| Reaction temperature/DEG C | 320-340 |
| Volume space velocity/h-1 | 1.0 |
| Hydrogen to oil volume ratio | 600 |
Table 2
| Project | Data |
| Kinematic viscosity (100 DEG C)/(mm2/s) | 5.8 |
| Condensation point/DEG C | 46 |
| Sulfur content/(μ g/g) | <10 |
| Nitrogen content/(μ g/g) | <5 |
Table 3 generates oily (>=420 DEG C of fractions) property
Liquid receipts refer to：>=the yield of 420 DEG C of fractions is generated in oil, and computational methods are：(>=420 DEG C of fractions are generated in oil
Weight)/(in raw material >=420 DEG C of fraction weight).
By the result of table 3 and Fig. 1 it is found that the catalyst of the present invention is used for hydroisomerizing pour point depression for example for crude lube stock
When oily hydroisomerizing pour point depression, compared with contrast medium catalyst D1 and catalyst D2, the pour point for generating oil not only can be effectively reduced,
When identical pour point, the yield of high viscosity index (HVI) (VI) fluid product obviously increases.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of hydrogenation catalyst carrier, which is characterized in that the carrier includes：Composite molecular screen and heat-resistant inorganic oxide,
Wherein, the composite molecular screen is intersected the molecule screen banks of pore passage structure by the molecular sieve and two dimension of one-dimensional non-crossing pore passage structure
At the molecular sieve of the one-dimensional non-crossing pore passage structure is ZSM-22 molecular sieves, and the two dimension intersects the molecular sieve of pore passage structure
For beta-molecular sieve, the weight ratio that molecular sieve and the two dimension of one-dimensional non-crossing pore passage structure intersect the molecular sieve of pore passage structure is 6-9:
1, the aperture of the composite molecular screen is 5-20nm, pore volume 0.1-0.2ml/g, on the basis of the gross weight of carrier, compound point
The content of son sieve is 50-60 weight %.
2. carrier according to claim 1, wherein the heat-resistant inorganic oxide is aluminium oxide, amorphous silicon aluminium, oxidation
It is one or more in magnesium and boron oxide.
3. carrier according to claim 1, wherein the heat-resistant inorganic oxide is aluminium oxide and/or amorphous silicon aluminium.
4. a kind of hydrogenation catalyst, which is characterized in that the catalyst includes：Carrier and tool precious metal element with hydrogenation efficiency,
Wherein, the carrier is the carrier described in any one of claim 1-3.
5. catalyst according to claim 4, wherein on the basis of the gross weight of catalyst, the precious metal element, which accounts for, urges
The 0.1-1 weight % of agent total weight.
6. catalyst according to claim 4, wherein on the basis of the gross weight of catalyst, the precious metal element, which accounts for, urges
The 0.3-0.7 weight % of agent total weight.
7. according to the catalyst described in any one of claim 4-6, wherein the precious metal element is selected from the VIIIth expensive gold of race
Belong to one or more in element, the precious metal element exists with oxidation state and/or reduction-state.
8. catalyst according to claim 7, wherein the precious metal element is platinum and/or palladium.
9. the catalyst described in any one of carrier and claim 4-8 described in any one of claim 1-3 is adding
Application in hydrogen dewaxing.
10. catalyst described in any one of carrier and claim 4-8 described in any one of claim 1-3 containing
Application in wax stock oil Hydrodewaxing.
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| CN201410614427.0A CN105618155B (en) | 2014-11-04 | 2014-11-04 | Hydrogenation catalyst carrier and its application and hydrogenation catalyst and its application |
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| CN100425678C (en) * | 2005-01-14 | 2008-10-15 | 中国石油化工股份有限公司 | Dewaxing catalyst containing compound molecule sieve and preparation method thereof |
| CN100457867C (en) * | 2005-10-19 | 2009-02-04 | 中国石油化工股份有限公司 | Hydrodewaxing catalyst and its preparing method |
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