CN102309975B - Method for preparing hydrocracking catalyst - Google Patents
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- CN102309975B CN102309975B CN 201010222164 CN201010222164A CN102309975B CN 102309975 B CN102309975 B CN 102309975B CN 201010222164 CN201010222164 CN 201010222164 CN 201010222164 A CN201010222164 A CN 201010222164A CN 102309975 B CN102309975 B CN 102309975B
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Abstract
The invention discloses a method for preparing a hydrocracking catalyst, which comprises the following steps of: firstly, selecting powder of a hydrocracking catalyst carrier material which at least comprises one acid cracking material; then preparing metal salt solution containing hydrogenation active ingredients; impregnating the powder of the carrier material by the metal salt solution; filtering, drying and grinding the impregnated powder of the carrier material; adding a peptizer or an adhesion agent into the obtained product; carrying out molding after sufficiently grinding; and drying and roasting to obtain the catalyst product. The hydrocracking catalyst prepared by the method disclosed by the invention has high content of the hydrogenation active ingredients, also has larger porevolume, aperture and specific surface area and is more suitable for the hydrocracking process of heavy vacuum gas oil with a higher boiling point.
Description
Technical field
The present invention relates to the preparation method of a kind of preparation method's of hydrocracking catalyst, particularly heavy distillate hydrocracking catalyst.
Technical background
Hydrocracking technology has that adaptability to raw material is strong, production operation and characteristics such as the product solution flexibility is big, good product quality, various heavy inferior chargings can be converted into high-quality jet fuel, diesel oil, lube basestocks and chemical industry naphtha and the tail oil preparing ethylene by steam cracking raw material of market in urgent need, become one of modern oil refining and the most important heavy oil deep processing of petro chemical industry technology, obtained increasingly extensive application at home and abroad.
But because crude quality variation year by year, the sour crude of import increases considerably, and the refinery is for increasing economic efficiency, crude oil decompression deep drawing technology is generally adopted in beginning, make doing by original 520 ℃ of vacuum distillate bring up to about 600 ℃, impurity contents such as its density is increasing, boiling range is more and more higher, the molecular weight of contained hydrocarbon molecule is increasing, structure also becomes increasingly complex, sulphur nitrogen are also more and more, increased the difficulty of hydrocracking greatly, these are all had higher requirement to hydrocracking technology and hydrocracking catalyst.
Along with the raw material quality becomes heavy, variation, and the demand of product quality upgrading and device capacity expansion revamping promotes day by day, the refinery has proposed more and more higher requirement to the performance of hydrocracking catalyst, and the performance of the hydrocracking catalyst of common metal content (generally being lower than 30% in oxide hydrogenation metal total content) can not satisfy current actual user demand fully.Hydrocracking catalyst is the core of hydrocracking technology.The bifunctional catalyst that hydrocracking catalyst is made up of hydrogenating function and cracking function, wherein hydrogenating function is to be provided by hydrogenation active metals, improve the hydrogenation performance of hydrocracking catalyst, be conducive to the saturated of aromatic hydrocarbons, can make further open loop conversion of polycyclic aromatic hydrocarbon, this not only is conducive to handle the more hydrocracking raw material oil of heavy, poor quality, improve liquid product yield and produce high-quality hydrocracking product, can also further improve the ability of the anti-organic nitrogen poisoning of catalyst, reduce green coke, carbon deposit, prolong the service life of catalyst.Therefore, the hydrogenation performance of raising hydrocracking catalyst is to satisfy to handle inferior feedstock oil and produce the most important approach of high quality of products.
Usually the method that improves the hydrogenation performance of hydrocracking catalyst mainly contains to be improved catalyst interpolation auxiliary agent and improves hydrogenation metal content etc.The method of adding auxiliary agent mainly is by adding the active force that auxiliary agent improves carrier and hydrogenation metal, with the dispersion of raising hydrogenation metal on catalyst surface, and then the hydrogenation performance of raising catalyst.CN01123767.8 has provided a kind of hydrocracking catalyst preparation method who contains rare earth, and this method is improved the dispersity of carrier and hydrogenation metal by adding rare-earth additive, makes the hydrogenation performance of catalyst obtain certain improvement.US 6,527, and 945, CN00110016.5 and CN00109747.4 be by adding boron, phosphorus and halogen auxiliary agents such as (F, Cl), makes the performance of hydrocracking catalyst obtain further raising.But the method for adding auxiliary agent has just maximally utilised a limited number of hydrogenation sites, the hydrogenation performance of hydrocracking catalyst is significantly improved, improve hydrocracking catalyst hydrogenation metal content and can significantly improve the hydrogenation sites number, aspect hydrotreating catalyst, obtained extraordinary application.Introduce the employing coprecipitation method as patents such as patent US5086032, US4820677 and CN200410050730.9 and prepared high tenor hydrotreating catalyst, prepare tenor up to 50%～95% hydrotreating catalyst, the hydrogenation performance of catalyst has obtained great raising, and product quality has obtained great improvement.Though this type of catalyst has higher hydrogenation performance, but the catalyst pore volume is relative with specific area less, generally can only handle the following cut than lightweight of diesel oil, and since coprecipitation method to prepare the catalyst metals utilization rate low, metal dispersion can be bad, and complicated process of preparation, product stability is poor, so the catalyst cost performance is not high.Kneading method can prepare the catalyst of various active metallic contents, but the catalyst performance of kneading method preparation is relatively poor relatively, and the reactive metal effective rate of utilization is low, the less employing kneading method preparation of hydrogenation catalyst.US 5,565,088 has introduced a kind of NZMS of containing molecular sieve hydrocracking catalyst, adopt the immersion process for preparing catalyst, the catalyst that the catalyst of its high metal content is lower than tenor can be produced boat coal and the diesel product of better quality, do not surpass 40% but its tenor is the highest, product quality improves limited.
By above analysis, adopt the immersion process for preparing catalyst, can give full play to the performance of hydrogenation metal, but the tenor of preparation catalyst is very restricted; Though coprecipitation method can prepare the hydrotreating catalyst of high tenor, the utilization rate of metal is not high, and the catalyst pores structure also is subjected to certain restriction.Therefore, adopt the high metal of immersion process for preparing, and have large pore volume, bigger serface hydrocracking catalyst, will have very important Practical significance.
Summary of the invention
At the deficiency of existing common metal content hydrocracking catalyst performance and high tenor hydrocracking catalyst preparation method's restriction, the invention provides the preparation method of a kind of macropore, bigger serface, high tenor hydrocracking catalyst.
Hydrocracking catalyst preparation process of the present invention comprises following content:
(1) selective hydrocracking catalyst carrier material powder, carrier material comprise a kind of acid cracking material at least;
(2) preparation contains the metal salt solution of hydrogenation activity component, the hydrogenation activity component is generally one or more among W, Mo, Ni and the Co, with this metal salt solution impregnated carrier material powder, filtration then, dry, pulverizing, the hydrogenation activity component is dispersed in the carrier material powder;
(3) dispersion that obtains of step (2) the carrier material powder of hydrogenation activity component add peptizing agent or binding agent, fully roll aftershaping, dry, roasting obtains catalyst prod then.
Acid cracking material of the present invention comprises molecular sieve or amorphous acidic components, molecular sieve generally comprises one or more in Y zeolite, beta-molecular sieve, ZSM-5 molecular sieve, SAPO molecular sieve and the MCM-41 mesopore molecular sieve etc., and amorphous acidic components are generally one or more in amorphous aluminum silicide, amorphous silicon magnesium and the clay etc.Required molecular sieve can require the modification suit according to serviceability.Carrier material can also comprise acid more weak inorganic refractory oxide in the hydrocracking catalyst, is generally aluminium oxide or contains the auxiliary agent aluminium oxide, generally is raw material with the aluminum hydroxide solid elastomer powder when using.The raw material with large pore volume, bigger serface in preferred this area such as amorphous acidic components and aluminium oxide.By weight content in the final catalyst, the general content of acid carrier material is 1%～60%, the hydrogenation activity component is generally 35%～70% in the weight content of oxide in catalyst, is preferably 40%～60%, simultaneously can also be salic below 50%.
In the metal salt solution that contains the hydrogenation activity component in the step (2), can add suitable adjuvant component as required, as containing one or more the compound among P, F, B, Zr, the Ti etc. in the dipping solution.
Peptizing agent is generally acid solution in the step (3), and as rare nitric acid etc., binding agent is generally the little porous aluminum oxide through peptization.Moulding can determine according to the shape of final catalyst, as extrusion etc.The sintering temperature of catalyst is generally 300～600 ℃, and roasting time was generally 2～10 hours.
The hydrocracking catalyst of the inventive method preparation has following character, and specific area is 150m
2/ g～350m
2/ g is preferably 160m
2/ g～300m
2/ g; Pore volume is 0.20cm
3/ g～0.50cm
3/ g is preferably 0.30cm
3/ g～0.45cm
3/ g, the hydrogenation metal total content is 35%～70%, is preferably 40%～60%.
The inventive method adopts the method for carrier of hydrocracking catalyst material powder dipping hydrogenation activity component, compare with carrier impregnation after the moulding of routine, carrier material powder dipping can absorb more maceration extract, pick up than moulding after the carrier pick up improve several times.Therefore maceration extract does not need higher metal concentration just can prepare the higher final catalyst prod of active metallic content.Owing to do not need the dipping solution of high concentration, the solution preparation is simple, and stable in properties is fit to commercial scale and uses.Rarer slaine maceration extract can reduce the viscosity of solution, reduces solution surface tension, can weaken the influence of capillary resistance phenomenon in the dipping process like this.Can guarantee that not only metal component has higher content in the catalyst, can also further improve metal at the decentralization of carrier surface.The method of dipping hydrogenation component is compared after hydrocracking catalyst preparation method of the present invention and the carrier moulding, also help the aperture of when active metallic content is higher, improving final catalyst, after the conventional method carrier impregnation hydrogenation component, when particularly the hydrogenation component load capacity is big, the pore volume of catalyst, aperture and specific area all obviously reduce, even and during a large amount of hydrogenation component of the inventive method load, pore volume to final catalyst, aperture and specific area influence are less, can obtain hydrogenation component content height, large pore volume, bigger serface and wide-aperture hydrocracking catalyst.
In the preparation process of hydrocracking catalyst of the present invention, maceration extract can recycle.Therefore this method has characteristics such as preparation technology is simple, cost is low, pollution is little, and suitable commercial scale is promoted the use of.The catalyst of preparation goes for the more hydrocracking process of heavy, inferior raw material owing to have higher hydrogenation metal content and bigger pore volume and aperture.
The specific embodiment
A kind of detailed process of hydrocracking catalyst of the present invention is as follows:
(1) be example with tungsten nickel, non-your hydrogenation metal salting liquid preparation: get a certain amount of deionized water under stirring, add nickel nitrate and ammonium metatungstate crystal gradually, static after treating all to dissolve, filter, obtain metal impregnation solution, wherein WO
3Content 10.0～50.0gWO
3/ 100ml, NiO content 2.0～15.0gNiO/100ml.The preparation of molybdenum nickel, molybdenum cobalt and three constituent element metal component solution belongs to content well known to those skilled in the art.
(2) measure the contents on dry basis that hydrogenation splits catalyst carrier material, as the contents on dry basis of materials such as molecular sieve, aluminum hydroxide solid elastomer and the dried glue of amorphous aluminum silicide.Take by weighing a certain amount of said components in the required ratio of hydrocracking catalyst, place and stir metal impregnation solution, solid-to-liquid ratio is 1: 5～1: 20, and beating time is 30～120min.Mixed serum carries out suction filtration, and the filter cake butt is controlled 15%～30%, and drying is 2～6 hours under 100～150 ℃ of conditions, and the powder butt (weight) that contains the hydrogenation metal component is 40%～80%, pulverizes granularity control 100～200 orders then.
(3) powder of the dispersion hydrogenation metal component that (2) step is obtained rolls, and adding concentration behind 20～60min is 2～10gHNO
3/ 100ml dilute nitric acid solution continues to roll formation and can squeeze the paste shape, extruded moulding then, and catalyst shape can be column, clover, bunge bedstraw herb and other different in nature bar etc., length control 3～8mm.
(4) carrier strip that step (3) is obtained, at first under 100～150 ℃ of conditions dry 2～6 hours, carry out roasting then, 400～600 ℃ of sintering temperatures, the time is 2～10 hours, prepares the catalyst finished product.
Used modified molecular screen in the carrier of hydrocracking catalyst of the present invention can Modified Zeolite Y, one or more compound uses of beta-molecular sieve, ZSM-5 molecular sieve, SAPO molecular sieve and MCM-41 mesopore molecular sieve.The method of modifying of molecular sieve can be hydrothermal treatment consists or EDTA, SiCl
4, (NH
4)
2SiF
6, chemical dealuminization modification methods such as phosgene or oxalic acid, and the molecular sieve that uses method of modifying processing such as the hydro-thermal of acid, alkali, salt formula complexing agent combines with chemical dealuminization.The character of used modified molecular screen is: silica alumina ratio is 3～100, is preferably 10～60, Na
2O content≤0.5wt%, the meleic acid amount is 0.1～1.2mmol/g, preferred 0.2～0.6mmol/g.
Aluminium oxide or amorphous aluminum silicide that the present invention uses are generally selected super big hole modified aluminas and macropore amorphous aluminum silicide for use, can select existing goods, also can be according to prior art for preparing.The macropore modified aluminas of macroporous aluminium oxide such as CN200510047483.1 preparation, pore volume is up to 1.4mL/g～1.8mL/g, and specific area is 500m
2/ g～550m
2/ g.The high-silicon amorphous silica aluminum of amorphous aluminum silicide such as CN200810010246.1 preparation, pore volume is up to 1.0mL/g～2.0mL/g, and specific area is 400m
2/ g～650m
2/ g.
The present invention selects metallic salt solution for use, is generally group vib and VIII family metallic salt, and as the saline solution of metals such as W, Mo, Ni, Co one or more, metallic solution concentration is generally 5.0～50g metal/100mL.
The following examples are used for illustrating in greater detail the preparation method of carrier of the present invention, but scope of the present invention is not only limited to the scope of these embodiment.
The molecular sieve that uses among the embodiment as Modified Zeolite Y 1 as H type molecular sieve through the Modified Zeolite Y of 500 ℃ of hydrothermal treatment consists after 2 hours.Modified Zeolite Y 2 is the Modified Zeolite Y that Modified Zeolite Y 1 is handled through EDTA again.
The modified macroporous aluminum oxide dry glue powder of silicon of aluminum hydroxide solid elastomer powder 1:CN200510047483.1 embodiment 10 preparations of using among the embodiment.Aluminum hydroxide solid elastomer powder 2: sky, Tianjin company of a specified duration produces, 400 ℃ of roastings after 3 hours character be pore volume 0.82mL/g, specific area 323m
2/ g.
The amorphous aluminum silicide dry glue powder 1:CN200810010246.1 that uses among the embodiment implements the amorphous aluminum silicide dry glue powder of 9 preparations.The amorphous aluminum silicide dry glue powder of amorphous aluminum silicide dry glue powder 2:CN97116404.5 embodiment 8 preparations.
Embodiment 1
Contain Y molecular sieve 15% by final hydrocracking catalyst weight, contain amorphous aluminum silicide 25%, contain nickel oxide 12%, contain tungsten oxide 35%, surplus is that aluminium oxide is selected aforementioned Preparation of Catalyst raw material: modified Y molecular sieve 1, aluminum hydroxide solid elastomer powder 1 and amorphous aluminum silicide dry glue powder 1.
Catalyst preparation process is as follows: Y molecular sieve, aluminum hydroxide solid elastomer powder and amorphous aluminum silicide dry glue powder are fully mixed, the solution hybrid infusion making beating that contains hydrogenation component nickel and tungsten compound with preparation, dip time 120min, suction filtration, drying is 4 hours under 120 ℃, pulverize then, with 180 orders sieve powder.Powder is mixed with an amount of extrusion aid sesbania powder, and adding concentration is 4gHNO
3Rare nitric acid of/100ml carries out peptization, and being extruded into diameter is 1.5mm clover strip.Descended dry 4 hours at 120 ℃ then, 480 ℃ of following roastings 3 hours, the catalyst numbering was respectively HC-1.
Embodiment 2
Contain Y molecular sieve 25% by final hydrocracking catalyst weight, contain amorphous aluminum silicide 10%, contain nickel oxide 10%, contain tungsten oxide 30%, surplus is that aluminium oxide is selected aforementioned Preparation of Catalyst raw material: modified Y molecular sieve 1, aluminum hydroxide solid elastomer powder 1 and amorphous aluminum silicide dry glue powder 2.
The preparation method obtains catalyst and is numbered HC-2 with embodiment 1.
Embodiment 3
Contain Y molecular sieve 30% by final hydrocracking catalyst weight, contain amorphous aluminum silicide 10%, contain nickel oxide 10%, contain tungsten oxide 30%, surplus is that aluminium oxide is selected aforementioned Preparation of Catalyst raw material: modified Y molecular sieve 1, aluminum hydroxide solid elastomer powder 2 and amorphous aluminum silicide dry glue powder 1.
The preparation method obtains catalyst and is numbered HC-3 with embodiment 1.
Embodiment 4
Contain Modified Zeolite Y 5% by final hydrocracking catalyst weight, amorphous aluminum silicide 38%, contain nickel oxide 12%, contain tungsten oxide 43% and select aforementioned Preparation of Catalyst raw material: modified Y molecular sieve 2, aluminum hydroxide solid elastomer powder 1 and amorphous aluminum silicide dry glue powder 1, contain phosphoric acid in the dipping solution, contain 2% phosphorous oxides in the final catalyst.
The preparation method obtains catalyst and is numbered HC-4 with embodiment 1.
Comparative example 1
Catalyst according to embodiment 1 is formed and raw material, earlier support material is made catalyst carrier, infusion process load hydrogenation activity component is adopted in the base back, need carry out twice active metal component dipping and just must obtain required active metallic content, is numbered HC-B1 to catalyst.
Comparative example 2
Catalyst according to embodiment 4 is formed and raw material, earlier support material is made catalyst carrier, infusion process load hydrogenation activity component is adopted in the base back, need carry out twice active metal component dipping and just must obtain required active metallic content, is numbered HC-B2 to catalyst.
In the present embodiment, above each routine catalyst is carried out instrumental analysis and activity rating.Each routine catalyst physico-chemical property is shown in Table 1.
Table 1. catalyst physico-chemical property
Annotate: R
BETAverage pore diameter for BET method mensuration.
Evaluating apparatus adopts on the 200ml small hydrogenation device and carries out, and before the activity rating catalyst is carried out presulfurization.The raw materials used oil nature of evaluation of catalyst activity and reaction process condition see Table 2 and table 3, and the catalyst reaction performance comparison the results are shown in Table 4.When estimating HC-1, HC-2, HC-3 and HC-B1, feedstock oil directly enters the hydrocracking catalyst bed then through the Hydrobon catalyst bed earlier, and the organic nitrogen content during through the Hydrobon catalyst bed in the control feedstock oil is lower than 20 μ g/g.When estimating HC-4 and HC-B2, do not use the Hydrobon catalyst bed, feedstock oil is directly by the hydrocracking catalyst bed.
Table 2. feedstock oil character
Table 3. evaluating catalyst process conditions
Table 4. catalyst reaction performance comparison result
Table 5 catalyst reaction performance comparison result
Annotate: intermediate oil comprises kerosene distillate and diesel oil distillate.
Claims (7)
1. the preparation method of a hydrocracking catalyst, its preparation process comprises following content:
(1) selective hydrocracking catalyst carrier material powder, carrier material comprise a kind of acid cracking material at least;
(2) preparation contains the metal salt solution of hydrogenation activity component, the hydrogenation activity component is one or more among W, Mo, Ni and the Co, with this metal salt solution impregnated carrier material powder, filtration then, dry, pulverizing, the hydrogenation activity component is dispersed in the carrier material powder;
(3) dispersion that obtains of step (2) the carrier material powder of hydrogenation activity component add peptizing agent or binding agent, fully roll aftershaping, dry, roasting obtains catalyst prod then;
By weight content in the final catalyst, the acid carrier material content is 1%～60%, and the hydrogenation activity component is 40%～70% in the weight content of oxide in catalyst.
2. it is characterized in that in accordance with the method for claim 1: acid cracking material comprises molecular sieve or amorphous acidic components.
3. in accordance with the method for claim 2, it is characterized in that: molecular sieve comprises one or more in Y zeolite, beta-molecular sieve, ZSM-5 molecular sieve, SAPO molecular sieve and the MCM-41 mesopore molecular sieve, and amorphous acidic components are one or more in amorphous aluminum silicide, amorphous silicon magnesium and the clay.
4. it is characterized in that in accordance with the method for claim 1: the hydrogenation activity component is 40%～60% in the weight content of oxide in catalyst.
5. in accordance with the method for claim 1, it is characterized in that: in the metal salt solution that contains the hydrogenation activity component in the step (2), contain among auxiliary agent P, F, B, Zr, the Ti one or more compound.
6. in accordance with the method for claim 1, it is characterized in that: peptizing agent is acid solution in the step (3), and binding agent is the little porous aluminum oxide through peptization.
7. in accordance with the method for claim 1, it is characterized in that: the sintering temperature of catalyst is 300～600 ℃, and roasting time is 2～10 hours.
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| CN106582738B (en) * | 2016-12-15 | 2020-01-03 | 中国海洋石油集团有限公司 | Hydrofining catalyst and preparation method thereof |
| CN106622314B (en) * | 2016-12-15 | 2020-01-07 | 中国海洋石油集团有限公司 | High-activity hydrofining catalyst and preparation method thereof |
| CN110038622B (en) * | 2018-01-16 | 2021-12-07 | 中国石油化工股份有限公司 | Hydrocracking catalyst and preparation method thereof |
| CN114471669B (en) * | 2020-10-27 | 2023-07-28 | 中国石油化工股份有限公司 | Hydrocracking catalyst and preparation method and application thereof |
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