CN1224458C - Process for preparing hydrocracking catalyst - Google Patents
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- CN1224458C CN1224458C CN 01119819 CN01119819A CN1224458C CN 1224458 C CN1224458 C CN 1224458C CN 01119819 CN01119819 CN 01119819 CN 01119819 A CN01119819 A CN 01119819A CN 1224458 C CN1224458 C CN 1224458C
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Abstract
The present invention provides a method for preparing a petroleum hydrocarbon hydrocracking catalyst, which includes the following steps: firstly, forming a catalyst carrier, and then post-treating the catalyst carrier by aqueous solution containing an ammonium salt and acid. When used for preparing the hydrocracking catalyst, the method has the advantages of simple preparation method, convenient operation, low cost and good combination property of catalyst.
Description
The petroleum hydrocarbon hydrocracking technology is to depress at higher hydrogen branch, hydrocarbon molecules and hydrogen carry out cracking and hydrogenation reaction at catalyst surface, generate the conversion process of less molecule, can adopt heavy distillate, comprise catalytic cracking recycle oil and coker distillate etc., production high-quality oil product, particularly production high-quality aviation kerosine and low freezing point diesel fuel, it is strong to have adaptability to raw material, light-end products yield height, characteristics such as quality is good, operating flexibility is big in addition, can adopt different operating conditions, produce kerosene as required, diesel oil, gasoline direct is to isopentane and isohexane etc.
The key of hydrocracking technology is a catalyst.Hydrocracking catalyst is typical bifunctional catalyst, is made up of cracking function (acid carrier) and hydrogenating function (metal component).The metal component of industry hydrocracking catalyst generally is base metal (Ni, Co, Mo, a W) sulfide.Acid carrier mainly contains: SiO
2-Al
2O
3, SiO
2Amorphous component and molecular sieves such as-MgO; And the character of acidic components plays crucial effects to catalyst performance.The non-framework aluminum that midbarrel oil type hydrocracking catalyst requires molecular sieve to have high silica alumina ratio, high-crystallinity, large aperture, big secondary pore pore volume and quantitatively can control.Because this molecular sieve acid site density is low, total acid content is few, and alkali metal can make the acid site poison, so the alkali-metal content in the catalyst is wanted strict restriction, Na
2The general requirement of O content is lower than 0.1%, even wishes Na
2O content is lower than 0.05%.So low alkali metal content has very high requirement to the preparation of molecular sieve modified method, amorphous aluminum silicide and activated alumina, must increase roasting and ammonium exchange number of times with further reduction alkali metal content, increased the catalyst cost greatly, improved requirement production equipment.
Chinese patent CN1179400A has described a kind of preparation method who is used for the molecular sieve of hydrocracking catalyst.For Na with molecular sieve
2O% content is reduced to below 0.1%, needs ammonium exchange 12 times, and production efficiency is very low, and does not see the Na in the catalyst carrier
2The O% content data.
USP3,402,996 have described a kind of preparation method of molecular sieve, for making the Na of USY molecular sieve
2O% content is controlled at below 0.3%, be with molecular sieve ammonium exchange 5 times, then through 816 ℃ of roastings, the structure that the back single stepping can the grievous injury molecular sieve wherein, thereby reduce crystallization reservation degree greatly, to how with the Na of molecular sieve
2O% content is reduced to below 0.1%, does not provide concrete grammar.
The acidic components that use in the hydrocracking catalyst also comprise amorphous aluminum silicide and alumina component except that molecular sieve.
Wherein the preparation as the activated alumina of acid carrier has following several method:
The aluminium hydroxide secondary precipitation.No matter be that acid solution method (aluminum nitrate+NaOH method) (US4,188,881) or aqueous slkali method (sodium metaaluminate+salt acid system) (US 4,102,818) all need aluminum hydroxide precipitation is got off, filter flushing.Alkali metal cation contains in aluminum hydroxide precipitation, just alkali metal content can be lowered through repeatedly washing, and general aluminum hydroxide precipitation is difficult to filter, and the operation cycle of practical operation is long, and work efficiency is low, produces a large amount of industrial wastewaters in addition;
Adopt aluminium alcoholates Hydrolyze method (US 2,682,246, and US 4,202,870 etc.), can obtain the activated alumina that the very high specific surface of purity is big, voidage is high.This method has obtained industrialization, adopts metallo-organic compound (aluminium alcoholates) but the shortcoming of this method is an initiation material, must adopt special equipment production also to produce large amount of sewage, and the cost of the aluminium oxide that obtains of this method is very high.
The preparation amorphous aluminum silicide is similar with the situation of preparation aluminium hydroxide, owing to filter difficulty more, very difficult alkali-metal content is reduced to satisfied the hydrocracking catalyst performance demands.
Because the cost height of material therefor, the price of corresponding industrial hydrocracking catalyst is also higher.In addition, alkali-metal existence has reduced the performance of catalyst, is difficult to satisfy the requirement of hydrocracking technology development to catalyst performance, has restricted development of technologies.
In order to improve catalyst performance, Chinese patent CN1056514A has described a kind of processing method of carrier of hydrocracking catalyst, and with ammonium fluoride solution impregnation catalyst agent carrier, the content of the fluorine ion of increase carrier is to improve support acidity, catalyst activity increases, but amplitude and little.
The preparation method who the purpose of this invention is to provide a kind of petroleum hydrocarbon hydrocracking catalyst can regulate the content of alkali metal ion in the catalyst effectively according to this method.When adopting this method to prepare hydrocracking catalyst, the preparation method is simple, and is easy to operate, and cost is low, and the catalyst good combination property.
The preparation method of petroleum hydrocarbon hydrocracking catalyst provided by the invention comprises:
(1) molecular sieve and aluminium hydroxide and/or amorphous aluminum silicide and peptizing agent are mixed pinch or extrusion is shaped, and drying and roasting, the catalyst carrier that obtains being shaped;
(2) catalyst carrier that gained is shaped is handled with the aqueous solution that contains ammonium salt and is made its Na
2O content is reduced to below the 0.2 weight %;
(3) with (2) gained catalyst carrier at 350-550 ℃ of roasting 0.5-4 hour;
(4) with the hydrogenation metal active component of (3) gained catalyst carrier according to requirement in the conventional method load.
Method provided by the invention is characterised in that earlier catalyst carrier is shaped that the carrier after will being shaped is then handled and made its sodium oxide content be reduced to desired horizontal, rather than adopts the method for falling sodium, postforming earlier as prior art.There is not the problem of filtration difficulty in carrier after owing to be shaped, does not need that sodium is separately fallen in molecular sieve and aluminium oxide or amorphous aluminum silicide yet and handles, and has so just simplified operation greatly, and operation becomes simple and easily.As for composition, shape, the manufacturing process of catalyst, the selection of falling sodium method, hydrogenation metal active component (as Ni, Co, Mo, W etc.) and carrying method etc., can select according to prior art, the present invention has no particular limits it.
For example, the said molecular sieve of step in the method provided by the invention (1) is generally Y zeolite, also can be the mixture of Y zeolite and β zeolite, modenite, MCM-41 etc.; Described Y zeolite can be the Y zeolite that has exchanged processing and/or super stabilizing processing through preliminary ammonium, and its lattice constant scope can be the 2.420-2.460 nanometer, but does not require that its sodium oxide content is lower than 0.1 weight %.Said amorphous aluminum silicide and aluminium hydroxide can be respective material well known in the art, and for example silica alumina ratio is amorphous aluminum silicide, boehmite, boehmite, gibbsite, surge aluminium stone of 2-10 etc.Described peptizing agent can be inorganic acid such as nitric acid, hydrochloric acid, also can be organic acid such as formic acid, acetate, citric acid, oxalic acid, malonic acid, tartaric acid etc.Described manufacturing process can be compression forming, extrusion molding, rotational forming, spray shaping etc.The cross sectional shape of formed catalyst can be round, quadrangle, triangle, cloverleaf pattern, bunge bedstraw herb shape etc.; It also can be the distortion of these shapes.When shaped catalyst, can also add extrusion aid such as sesbania powder.More particularly, the manufacturing process of catalyst carrier can be: with molecular sieve and amorphous aluminum silicide and/or aluminium hydroxide according to molecular sieve: amorphous aluminum silicide and/or aluminium hydroxide=1: ratio (0.6-5) mixes, add an amount of peptizing agent, mix the back machine shape, oven dry back is 300-650 ℃ roasting temperature 2-3 hour, the catalyst carrier that obtains being shaped.
Step in the method provided by the invention (2) is said to be handled and can carry out according to the conventional method of molecular sieve ammonium exchange with ammonium salt aqueous solution, be that 0.1-2M, consumption are that the 3-10 ammonium salt aqueous solution doubly of described catalyst carrier weight ℃ was handled 0.2-2 hour down in room temperature to 100 for example with concentration, the solution that anhydrates that can incline after the processing adds entry and cleans; Describedly handle and the water cleaning can be carried out repeatedly, until the Na that makes catalyst carrier with ammonium salt aqueous solution
2O content is reduced to below the 0.1 weight %.After the carrier oven dry that will handle then, 350-550 ℃ of roasting 0.5-4 hour (step (3)).
The used ammonium salt of step (2) can be an inorganic ammonium salt, as ammonium nitrate, ammonium chloride, ammonium sulfate, ammonium fluoride, carbonic hydroammonium, ammonium phosphate, also can adopt organic acid ammonium salt such as ammonium acetate, ammonium oxalate, ammonium citrate, ammonium tartrate etc., also can be any mixing of above-mentioned various components.
When the ammonium salt solution that carries out step (2) was handled, described ammonium salt solution can optionally contain acid, and to make the pH of solution when handling be 2.5-6.Used acid can be organic acid, for example ethylenediamine tetra-acetic acid, oxalic acid, sulfosalicylic acid etc.; Also can be inorganic acids, for example hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid etc.
The described hydrogenation metal active component with requirement in the load of gained catalyst carrier of step in the method provided by the invention (4) is carried out according to the method for prior art, described hydrogenation metal active component can be selected from one or more among Ni, Co, Mo, the W, its load capacity is selected according to the actual industrial needs, and the present invention has no particular limits it.The load of reactive metal can be adopted saturated infusion process, also can adopt the supersaturation infusion process.All reactive metals on can single-steeping also can flood several times.When employing is repeatedly flooded, flood between two kinds of metal steps and can carry out roasting, also can not carry out roasting.But generally need be after all reactive metal dippings are finished with the roasting according to a conventional method of gained catalyst.The load capacity of described reactive metal has no particular limits, and is generally the 10-35 weight % of total catalyst weight.
In order to be illustrated more clearly in the present invention, list following examples, but can not be interpreted as it is restriction scope of the present invention.
Comparative Examples 1
Do not take off the Preparation of catalysts that sodium is handled after carrying out after this Comparative Examples explanation carrier is shaped.
(the Lanzhou catalyst plant is produced, and lattice constant is 2.439 nanometers, and degree of crystallinity is 78.9%, Na to get the high-silicon Y-Zeolite raw material
2O content is 0.68 weight %, down together) 300g, boehmite powder (Shandong Aluminum Plant's commodity, Na
2O content is 0.43 weight %, down together) 450g, amorphous aluminum silicide (produce, SiO by the Lanzhou Oil Refinery catalyst plant
2/ Al
2O
3Mol ratio is 4.5, Na
2O content is 0.21 weight %, 750g down together), sesbania powder 10g mixes, and adds 1200 milliliters of 3% aqueous solution of nitric acid gradually, be in harmonious proportion evenly, be extruded into the cylindrical bar that diameter is 2.2mm with banded extruder, with it in 120 ℃ of down oven dry 4 hours, 550 ℃ of following roastings 3 hours in Muffle furnace then, the catalyst carrier that obtains being shaped is designated as carrier a.
Getting nickel nitrate 34g adds to 30ml and contains WO
3In the ammonium metatungstate solution of 120g/ml, add water to 100ml, stir, be prepared as metal impregnation and tuck in; Get carrier a 100g, place maceration extract, flooded 2 hours, then in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace again obtain catalyst A.
Comparative Examples 2
The Preparation of catalysts of sodium postforming is taken off in the explanation of this Comparative Examples earlier.
Get high-silicon Y-Zeolite raw material 200g, join the NH that 3000ml concentration is 0.7M
4In the Cl aqueous solution, stirred 2 hours down, filter, be washed to no Cl in 90 ℃
-Similarity condition and step be repeated exchanged 7 times again, oven dry then, the y-type zeolite that obtains by analysis, recording its lattice constant is 2.439 nanometers, degree of crystallinity is 79.4%, Na
2O content is 0.08 weight %.
Get the above-mentioned Y zeolite 300g that takes off behind the sodium, boehmite 450g, amorphous aluminum silicide 750g, sesbania powder 10g mixes, add 3% aqueous solution of nitric acid 1200ml gradually, be in harmonious proportion evenly, be extruded into the cloverleaf pattern bar that diameter is 1.8mm, it was dried 4 hours down in 120 ℃ with banded extruder, 550 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst carrier b.Getting nickel nitrate 34g adds to 30ml and contains WO
3In the ammonium metatungstate solution of 120g/ml, add water to 100ml, stir, be prepared as the metal mixed maceration extract, get catalyst carrier b 100g, place this maceration extract, flooded 2 hours, in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst B
Embodiment 1
With 132 gram (NH
4)
2SO
4Be dissolved in the 1000ml water, drip 0.5N hydrochloric acid and make that its pH value is 3.0, heat temperature raising to 90 ℃, the carrier a 120g that will prepare according to the same procedure of Comparative Examples 1 adds in this aqueous solution, stirs 1.5 hours, and the solution that anhydrates inclines; Add deionized water 1000ml, be warming up to 90 ℃, stirred 2 hours, the solution that anhydrates that inclines is washed 2 times with quadrat method again, dries 2 hours down for 120 ℃.The carrier of drying is handled once and washed 2 times with ammonium salt solution again according to above-mentioned condition and step, 120 ℃ of oven dry 4 hours down, 450 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst carrier.
Getting nickel nitrate 34g joins 30ml and contains WO
3In the ammonium metatungstate aqueous solution of 120g/ml, add water to 100ml, stir, make metal impregnation liquid, get the catalyst carrier 100g after the above-mentioned processing, place this maceration extract, flooded 2 hours, in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst C.
Embodiment 2
With 1000ml concentration is the NH of 0.5M
4Cl aqueous solution heat temperature raising to 90 ℃ will join in this aqueous solution according to the carrier a 120g of the same procedure preparation of Comparative Examples 1, stirs 1.5 hours, and the solution that anhydrates that inclines is according to using NH again with quadrat method
4Cl solution-treated 3 times, then in 120 ℃ of down oven dry 2 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst carrier.
Getting nickel nitrate 34g joins 30ml and contains WO
3In the ammonium metatungstate solution of 120g/ml, add water to 100ml, stir, make metal impregnation and tuck in, get the catalyst carrier 100g after the above-mentioned processing, place maceration extract, flooded 2 hours, in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst D.
Embodiment 3
In 1000ml concentration is the NH of 0.2M
4Add ammonium fluoride 20g in the Cl aqueous solution, agitating heating is warming up to 90 ℃, and the carrier a 120g that will prepare according to the same procedure of Comparative Examples 1 joins in this aqueous solution then, stirred 2 hours, the solution that anhydrates that inclines adds deionized water 1000ml, is warming up to 90 ℃, stirred 2 hours, the solution that anhydrates that inclines is used ammonium salt solution and water treatment totally 3 times so repeatedly, with it 120 ℃ of oven dry 4 hours down, 500 ℃ of following roastings 2 hours in Muffle furnace then obtain catalyst carrier.
Getting nickel nitrate 34g joins 30ml and contains WO
3In the ammonium metatungstate solution of 120g/ml, add water to 100ml, stir, make metal impregnation and tuck in, get the catalyst carrier 100g after the above-mentioned processing, place maceration extract, flooded 2 hours, in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst E.
Embodiment 4
Get NH
4Y zeolite raw material (produce, and lattice constant is 2.456 nanometers, and degree of crystallinity is 82.9%, Na by Chang Ling oil plant catalyst plant
2O content is 3.65 weight %) 300g, boehmite powder 1200g, sesbania powder 10g mixes, and adds 1200 milliliters of 3% aqueous solution of nitric acid gradually, be in harmonious proportion evenly, be extruded into the cloverleaf pattern bar that diameter is 1.8mm with banded extruder, with it in 120 ℃ of down oven dry 4 hours, 550 ℃ of following roastings 3 hours in Muffle furnace then, the catalyst carrier that obtains being shaped is designated as carrier c.
In 1000ml concentration is the NH of 0.5M
4Splash into 0.5N hydrochloric acid in the Cl aqueous solution, to the pH value be 4.5, heat temperature raising to 90 ℃ adds above-mentioned carrier c 120g in this aqueous solution, stirs 1.5 hours; The solution that anhydrates that inclines adds deionized water 1000ml, is warming up to 90 ℃, stirs 2 hours, and the solution that anhydrates that inclines is washed once with quadrat method again; 120 ℃ down oven dry after 2 hours the carrier of drying is handled and washing with ammonium salt solution according to above-mentioned condition and step again, repeat altogether 3 times, 120 ℃ of oven dry 4 hours down, 450 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst carrier.
Getting nickel nitrate 34g joins 30ml and contains WO
3In the ammonium metatungstate solution of 120g/ml, add water to 100ml, stir, make metal impregnation and tuck in, get the catalyst carrier 100g after the above-mentioned processing, place this maceration extract, flooded 2 hours, in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst F.
Embodiment 5
In 1000ml concentration is to add oxalic acid 35g in the ammonium oxalate aqueous solution of 0.2M, stirs, and heat temperature raising to 90 ℃ treats that all components all dissolves, and will add in this aqueous solution according to the carrier a 120g of the same procedure preparation of Comparative Examples 1, stirs 2 hours, and the solution that anhydrates inclines; Add deionized water 1000ml, be warming up to 90 ℃, stirred 2 hours, the solution that anhydrates inclines; Handle and washing with ammonium salt aqueous solution with quadrat method, reprocessing is 3 times altogether again; Then in 120 ℃ of down oven dry 4 hours, 450 ℃ of following roastings 3 hours in Muffle furnace again obtain catalyst carrier.
Getting nickel nitrate 34g joins 30ml and contains WO
3In the ammonium metatungstate solution of 120g/ml, add water to 100ml, stir, make metal impregnation liquid, get the catalyst carrier 100g after the above-mentioned processing, place maceration extract, flooded 2 hours, in 120 ℃ of down oven dry 4 hours, 500 ℃ of following roastings 3 hours in Muffle furnace then obtain catalyst G.
The sodium oxide content of the various embodiments described above and Comparative Examples gained catalyst is as shown in table 1.Though the sodium content of the catalyst molecular sieve wherein of Comparative Examples 2 gained is lower as can be seen, because the sodium in boehmite and the amorphous aluminum silicide does not remove, the sodium content of gained catalyst prod is still higher.
The Na of table 1, catalyst
2O content
| Catalyst | A | B | C | D | E | F | G |
| Na 2O, weight % | 0.42 | 0.30 | 0.09 | 0.10 | 0.14 | 0.17 | 0.07 |
Embodiment 6
The hydrocracking reaction performance of present embodiment explanation catalyst.
The evaluating catalyst condition:
Catalyst amount, 0.15g (60-80 order), with the dilution of 0.3g quartz sand, beds is up and down all with quartz sand filling, tube inner diameter 8mm, long 320mm, constant temperature head of district 20mm (catalyst practical application 10mm).
Reaction condition: adopt 6%CS earlier
2/ n-hexane was in 300 ℃ of presulfurizations 2 hours.Being warming up to 360 ℃, is the model compound evaluate catalysts with n-decane (nC10), nC10 flow velocity 0.1ml/min, H
2Flow velocity 400ml/min represents catalyst activity with the n-decane conversion ratio, represents the isomery performance of catalyst with isomerized products yield under the same conversion, and product is through the gas-chromatography on-line analysis.Chromatographic condition: fixer OV-101, carrier are silanization 201 red supporters, and fixer is coated with stain amount 15%, stainless steel chromatogram post, internal diameter 2mm, external diameter 3mm, length 3.8m.Fid detector, N
2Flow velocity 30ml/min, 210 ℃ of vapourizing temperatures, 210 ℃ of detector temperatures, quantity tube sampling, on-line analysis.Analysis condition: 40 ℃ of constant temperature 2min, 20 ℃/min temperature programming to 160 ℃, constant temperature 6min.
Each activity of such catalysts situation is as shown in table 2:
Table 2, catalyst performance are relatively
| Catalyst | Conversion ratio % * | Isomerized products yield % ** |
| A B C D E F G | 38.8 42.2 62.3 61.1 61.9 77.3 73.5 | 3.5 3.1 2.65 2.6 2.6 2.0 2.45 |
* the conversion ratio under 360 ℃.
* isomerized products yield all adopts numerical value under the same conversion.Concrete grammar is that conversion ratio and isomerized products yield are figure, get equally under 60% conversion ratio the isomerized products yield.
By the catalyst performance comparable situation of table 2 as can be seen, the performance of catalyst is relevant with the sodium oxide content of carrier, and sodium oxide content is high more, and catalyst activity is low more.The catalyst that wherein adopts ammonium/acid-treated catalyst (C), adds ammonium fluoride (E) and adopt oxalic acid/ammonium oxalate method (G) preparation, active increase rate is big, and isomery performance height.Adopt the first moulding of the present invention method of post processing again, not only simple to operately easily and be easier to reduce the sodium content of catalyst, improve the combination property of catalyst.
Claims (6)
1, a kind of preparation method of petroleum hydrocarbon hydrocracking catalyst is characterized in that this method comprises:
(1) molecular sieve and aluminium hydroxide and/or amorphous aluminum silicide are mixed pinch or extrusion is shaped, and drying and roasting, the catalyst carrier that obtains being shaped;
(2) catalyst carrier that gained is shaped is handled with the aqueous solution that contains ammonium salt and is made its Na
2O content is reduced to below the 0.2 weight %;
(3) with (2) gained catalyst carrier at 350-550 ℃ of roasting 0.5-4 hour;
(4) with the hydrogenation metal active component of requirement in the load of (3) gained catalyst carrier.
2, according to the process of claim 1 wherein that said molecular sieve is a Y zeolite.
3, according to the method for claim 1, wherein the used ammonium salt of step (2) is the inorganic ammonium salt that is selected from ammonium nitrate, ammonium chloride, ammonium sulfate, ammonium fluoride, carbonic hydroammonium or the ammonium phosphate, perhaps be the organic acid ammonium salt that is selected from ammonium acetate, ammonium oxalate, ammonium citrate or the ammonium tartrate, or the combination of these ammonium salts.
4, according to the method for claim 1, wherein the said aqueous solution that contains ammonium salt of step (2) optionally contains acid to make the pH of solution when handling is 2.5-6, used acid is the organic acid that is selected from ethylenediamine tetra-acetic acid, oxalic acid or the sulfosalicylic acid, perhaps for being selected from the inorganic acid in hydrochloric acid, sulfuric acid, nitric acid or the phosphoric acid.
5, according to the process of claim 1 wherein that the said aqueous solution that contains ammonium salt of step (2) is the aqueous solution that contains ammonium oxalate and oxalic acid.
6, according to the process of claim 1 wherein that said hydrogenation metal active component is to be selected among Ni, Co, Mo, the W one or more.
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| CN 01119819 CN1224458C (en) | 2001-06-29 | 2001-06-29 | Process for preparing hydrocracking catalyst |
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|---|---|---|---|
| CN 01119819 CN1224458C (en) | 2001-06-29 | 2001-06-29 | Process for preparing hydrocracking catalyst |
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| CN102309975B (en) * | 2010-07-07 | 2013-10-09 | 中国石油化工股份有限公司 | Method for preparing hydrocracking catalyst |
| CN102309971B (en) * | 2010-07-07 | 2013-11-20 | 中国石油化工股份有限公司 | Preparation method for hydro-treating catalyst |
| CN104043473B (en) * | 2013-03-13 | 2016-10-05 | 中国石油化工股份有限公司 | A kind of hydrocracking catalyst and application thereof |
| CN106669714B (en) * | 2015-11-11 | 2019-01-25 | 中国石油化工股份有限公司 | A kind of preparation method of hydrotreating catalyst |
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