CN1884446A - Hydrocracking catalyst for Tscher-Topsch synthesis of heavy wax, its preparation method and application thereof - Google Patents
Hydrocracking catalyst for Tscher-Topsch synthesis of heavy wax, its preparation method and application thereof Download PDFInfo
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- CN1884446A CN1884446A CN 200610012744 CN200610012744A CN1884446A CN 1884446 A CN1884446 A CN 1884446A CN 200610012744 CN200610012744 CN 200610012744 CN 200610012744 A CN200610012744 A CN 200610012744A CN 1884446 A CN1884446 A CN 1884446A
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Abstract
The invention relates the hydrogenation-cracking catalyst used to synthesize heavy wax, comprising 10.0-24.0wt% HY molecular screen, 10.0-24.0wt% SAPO-11 molecular screen, 3.0-10.0wt% nickel oxide, 3.0-10.0wt% nickel oxide, 0.0-15.0wt% molybdenum oxide or tungsten oxide, 10.0-24.0wt% amorphous oxide compound and 5.0-65.0wt% diaspore. The method comprises preparing carrier and dipping active component. The catalyst has the advantages of good catalytic cracking property, high diesel selective, and good isomerization property.
Description
Technical field
The invention belongs to a kind of hydrocracking catalyst and method for making thereof and application, relate in particular to a kind of hydrocracking catalyst and method for making and application that is applicable to Tscher-Topsch synthesis of heavy wax.
Technical background
In recent years, along with the atrophy of world's crude resources and raising up of crude oil price, energy consumption structure just changes to oil, coal and Sweet natural gas diversification gradually from oil dependent form, thereby makes coal/Sweet natural gas indirect liquefaction technology become one of the most attractive approach of back petroleum industry epoch liquid fuel.Coal is many, the few resource structures of oil and China has, by F-T synthetic with coal be converted into motor spirit be solve the present fuel oil shortage of China and clean, efficiently utilize one of the important channel of coal resources.
Hydrocracking technology is a kind of important refining of petroleum means, and its product has low-sulfur, hangs down the characteristics fragrant, that quality is high, is used widely in developed country.Fischer-Tropsch synthetic heavy hydrocarbon is compared with the oil heavy hydrocarbon, has the characteristics of no sulphur, no nitrogen, low virtue, and its organic hydrocarbon is mainly straight chain hydrocarbon.The C-C key bond energy of straight chain saturation alkane make comparatively difficulty of its selectivity scission of link, and condensation point is higher than equalization.Therefore how improving the selectivity of split product intermediate oil and the condensation point of reduction split product is the key of this catalyzer.
With the amorphous aluminum silicide is the hydrocracking catalyst of lytic activity component, in cracking process to wax, show intermediate oil selectivity preferably,, can obtain the diesel oil of highly selective by the adjusting of acidity, specific surface and secondary pore, but the catalyst hydrogenation cracking activity is low, running period short, reaction conditions is relatively harsher, and products obtained therefrom is based on straight-chain paraffin, although such diesel oil has higher cetane value, but its condensation point height needs further pour point depression and interpolation auxiliary agent to use.
The use of zeolite is a qualitative leap of hydrogen addition technology.It not only makes activity of such catalysts and election property significantly improve, and flexibility of operation is greatly strengthened, the more important thing is that it makes the isomer that some amount is arranged in the product of alkane cracking, therefore the full scale plant of present most of hydrocracking all uses the catalyzer that contains zeolite.Though it is the cracking performance of these catalyzer is stronger, when being applied to the hydrocracking of heavy hydrocarbon, relatively poor to the selectivity of middle distillate.
Because the relative merits complementation of amorphous oxide carrier and Zeolite support, according to the characteristic of two kinds of carriers and in the needs of oil type hydrocracking technology, select the complex carrier of two kinds of carriers can obtain result preferably as the carrier of hydrocracking catalyst.Can guarantee that so promptly the reactive behavior of catalyzer has improved the yield of intermediate oil again.
Industrial, zeolite molecular sieve also often mixes use with amorphous oxide and some binding agents, selects different zeolite contents according to the various objectives product.According to " Fuel Proceeing Technology " 1935:P55～85, for obtaining more gasoline component, then the content of zeolite in mixture is higher, can reach 80wt% in the heavy oit pyrolysis process; And when being the purpose product with diesel oil, then zeolite content is often between 5～15wt%.
Gortsema F G etc. reported once in US5047139 that with content be the Y zeolite (carrying through acidleach) of 7wt%, the SiO of 50wt%
2-Al
2O
3, 15wt% binding agent mix when supporting Ni-W, produce diesel oil efficient up to 87%, during than heavy oils component and macromole hydrocarbon, zeolite micropore has limited macromolecular diffusion, causes lytic activity to reduce for cracking.
The US4517074 patent disclosure a kind of hydrogenation crude catalyst for cracking, produce 150～370 ℃ intermediate oil, this catalyzer is except using zeolite component, its characteristics are to use a kind of Al
2O
3-SiO
2Dispersion system, its SiO
2Content reaches 20～65wt%, though the amorphous aluminum silicide in the dispersion system has certain lytic activity, but need be dispersed on certain alumina substrate, to carry the pore volume and the specific surface of a large amount of hydrogenation metal components, though this catalyzer has higher middle distillates oil selectivity, generally more than 80%, activity is lower, reach 60% transformation efficiency, temperature of reaction is generally more than 400 ℃.
SAPO series molecular sieve be 1984 by U.S. UCC company synthetic phosphate aluminium molecular sieve at first, its basic structural unit is PO
4, AlO
4And SiO
4Tetrahedron.Wherein SAPO-11 has the AEL configuration, belongs to rhombic system, and unit cell parameters is a=1.3425nm, b=1.8749nm, c=0.8429nm, and pore distribution concentration is at 0.6nm.Owing to contain P in the SAPO series molecular sieve, thus its acidity a little less than, the catalyzer that makes behind the loaded metal has good isomerization selectivity and activity to long chain alkane.
In EP300500, reported at least a silicoaluminophosphamolecular molecular sieves combined with the inorganic oxide matrix of 0～99wt% and made cracking catalyst, be used for the production of stop bracket gasoline.Many investigators use the SAPO-11 molecular sieve as the octane value growth promoter, its method mainly is that Y zeolite and SAPO-11 molecular sieve are mixed and made into catalyzer.Evaluation result shows, in catalyzer, add the SAPO-11 molecular sieve after, under all comparable condition of transformation efficiency and gasoline yield, aromaticity content or isomeric hydrocarbon all have raising with positive structure hydrocarbon ratio in the gasoline, infer that thus gasoline octane rating can corresponding increase.Find also that simultaneously low-carbon alkene content increases behind the adding SAPO-11 molecular sieve.
Summary of the invention
The purpose of this invention is to provide that a kind of activity is good, hydrocracking catalyst and the method for making and the application of isomery ratio height, Tscher-Topsch synthesis of heavy wax that the intermediate oil selectivity is high.
The hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax of the present invention is made up of nickel oxide, molybdenum oxide or Tungsten oxide 99.999, HY molecular sieve, SAPO-11 molecular sieve, pseudo-boehmite and amorphous oxide, the each component weight percent is: the HY type molecular sieve of 10.0～24.0wt%, 10.0 the SAPO-11 molecular sieve of～24.0wt%, 3.0 the nickel oxide of～10.0wt%, 0.0 the aluminum oxide of～15.0wt% or Tungsten oxide 99.999,10.0 the amorphous oxide of～24.0wt%, the pseudo-boehmite of 5.0～65.0wt%.
The step that the present invention prepares catalyzer is as follows:
(1) takes by weighing amorphous oxide, HY and SAPO-11 molecular sieve, behind binding agent pseudo-boehmite mixing, dilute nitric acid solution modulation, kneading and compacting with 5%, drying is 4～6 hours under 100～120 ℃, 4～6 hours postcooling of 500～600 ℃ of roasting temperatures obtain carrier to room temperature in air atmosphere then;
(2) adopt pickling process, the aqueous solution that will contain soluble molybdenum salt or soluble tungsten salt is impregnated on the carrier, evaporating solns is to doing under 100～120 ℃ condition, following dry 4～6 hours at 100～120 ℃ then, 500～600 ℃ of following roastings 4～6 hours, be cooled to room temperature, obtain the intermediates of loaded metal molybdenum or tungsten;
(3) carrier of intermediates that step (2) is obtained or step (1) preparation joins in the nickeliferous soluble salt solution, evaporating solns is to doing under 100～120 ℃ condition, following dry 4～6 hours at 100～120 ℃ then, 500～600 ℃ of following roastings 4～6 hours, be cooled to room temperature, obtain hydrocracking catalyst.
Containing soluble molybdenum salt as mentioned above is molybdate, preferred ammonium molybdate aqueous solution.
Nickeliferous as mentioned above soluble salt solution is carbonate or nitrate solution, the preferably nitrate aqueous solution.
Soluble tungsten salt is solubility metatungstate or ethyl metatungstate as mentioned above, preferred metatungstate.
Amorphous oxide is amorphous aluminum silicide, amorphous silicon magnesium and other modified aluminas etc. as mentioned above, preferred amorphous aluminum silicide.
Catalyzer of the present invention can be used for the hydrocracking process, is specially adapted to the process of Tscher-Topsch synthesis of heavy wax hydrocracking system intermediate oil, and its reaction conditions is: reaction pressure 3.0～10.0Mpa, hydrogen to oil volume ratio 400～1500, volume space velocity 0.5～2.0h
-1, 320～400 ℃ of temperature of reaction.
The present invention compared with prior art has the following advantages:
(1) catalyzer provided by the invention has good selectivity to middle distillate, helps the effective conversion of Tscher-Topsch synthesis of heavy wax to intermediate oil.
(2) catalyzer provided by the invention has good isomerization performance in hydrocracking, and the isomery selectivity of intermediate oil is higher.
The specific embodiment mode
Embodiment 1
(1) takes by weighing 26.0g HY molecular sieve, 13.0g SAPO-11 molecular sieve, 13.0g modified aluminas, after mixing with 48.0g binding agent pseudo-boehmite, dilute nitric acid solution modulation, kneading and compacting with 5%, with it 100 ℃ of following dry 6h in baking oven, 500 ℃ of roasting 6h postcooling just can obtain carrier of the presently claimed invention to room temperature.
(2) with the aqueous solution of nickelous nitrate as steeping fluid, to the carrier of moulding, evaporating solns is to doing under 100 ℃ condition with the solution impregnation of nickelous nitrate.With product dry 6h under 100 ℃, 500 ℃ of following roasting 6h postcooling are to room temperature, obtain the catalyzer of related use in the hydrocracking process of the present invention, wherein the mass percent of each component consists of: HY type molecular sieve 24.0wt%, SAPO-11 molecular sieve 12.0wt%, modified aluminas 12.0wt%, pseudo-boehmite 44.0wt%, nickel oxide 8.0wt%.
Pyroparaffine hydrocracking reaction conditions is: reaction pressure 5.0Mpa, hydrogen to oil volume ratio 1200, air speed 0.5h
-1, 360 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
Embodiment 2
(1) takes by weighing 13.0g HY molecular sieve, 13.0g SAPO-11 molecular sieve, 26.0g amorphous silicon magnesium, after mixing with 48.0g binding agent pseudo-boehmite, dilute nitric acid solution modulation, kneading and compacting with 5%, with it 110 ℃ of following dry 5h in baking oven, 550 ℃ of roasting 5h postcooling just can obtain carrier of the presently claimed invention to room temperature.
(2) with the aqueous solution of nickelous carbonate as steeping fluid, to the carrier of moulding, evaporating solns is to doing under 110 ℃ condition with the solution impregnation of nickelous carbonate.With product dry 5h under 110 ℃, 550 ℃ of following roasting 5h postcooling are to room temperature, obtain the catalyzer of related use in the hydrocracking process of the present invention, wherein the mass percent of each component consists of: HY type molecular sieve 12.0wt%, SAPO-11 molecular sieve 12.0wt%, amorphous silicon magnesium 24.0wt%, pseudo-boehmite 44.0wt%, nickel oxide 8.0wt%.
Pyroparaffine hydrocracking reaction conditions is: reaction pressure 3.0Mpa, hydrogen to oil volume ratio 1000, air speed 1.0h
-1, 400 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
Embodiment 3
(1) takes by weighing 13.0g HY molecular sieve, 26.0g SAPO-11 molecular sieve, 13.0g amorphous aluminum silicide, after mixing with 48.0g binding agent pseudo-boehmite, dilute nitric acid solution modulation, kneading and compacting with 5%, with it 120 ℃ of following dry 4h in baking oven, 600 ℃ of roasting 4h postcooling just can obtain carrier of the presently claimed invention to room temperature.
(2) with the aqueous solution of nickelous nitrate as steeping fluid, to the carrier of moulding, evaporating solns is to doing under 120 ℃ condition with the solution impregnation of nickelous nitrate.With product dry 4h under 120 ℃, 600 ℃ of following roasting 4h postcooling are to room temperature, obtain the catalyzer of related use in the hydrocracking process of the present invention, wherein the mass percent of each component consists of: HY type molecular sieve 12.0wt%, SAPO-11 molecular sieve 24.0wt%, amorphous aluminum silicide 12.0wt%, pseudo-boehmite 44.0wt%, nickel oxide 8.0wt%.
Pyroparaffine hydrocracking reaction conditions is: reaction pressure 9.0Mpa, hydrogen to oil volume ratio 800, air speed 1.5h
-1, 380 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
Embodiment 4
(1) takes by weighing 17.3g HY molecular sieve, 17.3g SAPO-11 molecular sieve, 17.3g amorphous aluminum silicide, after mixing with 48.0g binding agent pseudo-boehmite, dilute nitric acid solution modulation, kneading and compacting with 5%, with it 120 ℃ of following dry 5h in baking oven, 550 ℃ of roasting 6h postcooling just can obtain carrier of the presently claimed invention to room temperature.
(2) with the aqueous solution of nickelous nitrate as steeping fluid, to the carrier of moulding, evaporating solns is to doing under 110 ℃ condition with the solution impregnation of nickelous nitrate.With product dry 6h under 110 ℃, 550 ℃ of following roasting 6h postcooling are to room temperature, obtain the catalyzer of related use in the hydrocracking process of the present invention, wherein the mass percent of each component consists of: HY type molecular sieve 16.0wt%, SAPO-11 molecular sieve 16.0wt%, amorphous aluminum silicide 16.0wt%, pseudo-boehmite 44.0wt%, nickel oxide 8.0wt%.
Pyroparaffine hydrocracking reaction conditions is: reaction pressure 7.0Mpa, hydrogen to oil volume ratio 600, air speed 2.0h
-1, 320 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
Embodiment 5
Ammonium molybdate solution is impregnated on the shaping carrier among the embodiment 3, obtains containing the catalyzer of molybdenum, in 110 ℃ of dry 4h down, 550 ℃ of following roasting 5h; With the solution impregnation of nickelous nitrate to the catalyzer that contains molybdenum, dry 6h under 100 ℃, obtain the catalyzer of the related use of hydrocracking process of the present invention then in 600 ℃ of following roasting 4h, wherein the mass percent of each component consists of: HY type molecular sieve 10.5wt%, SAPO-11 molecular sieve 21.0wt%, amorphous aluminum silicide 10.5wt%, pseudo-boehmite 39.0wt%, nickel oxide 7.0wt%, molybdenum oxide 12.0wt%.
The pyroparaffine crack reacting condition is: reaction pressure 10.0Mpa, hydrogen to oil volume ratio 1500, air speed 1.5h
-1, 340 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
Embodiment 6
Sodium molybdate solution is impregnated on the shaping carrier among the embodiment 3, obtains containing the catalyzer of molybdenum, all the other preparation process are with embodiment 5.
The mass percent of catalyzer each component consists of: HY type molecular sieve 10.5wt%, SAPO-11 molecular sieve 21.0wt%, amorphous aluminum silicide 10.5wt%, pseudo-boehmite 39.0wt%, nickel oxide 7.0wt%, molybdenum oxide 12.0wt%.
The pyroparaffine crack reacting condition is: reaction pressure 10.0Mpa, hydrogen to oil volume ratio 1500, air speed 1.5h
-1, 340 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
Embodiment 7
Ammonium metatungstate solution is impregnated on the shaping carrier that obtains among the embodiment 3, obtains the catalyzer of tungstenic.All the other preparation process are with embodiment 5.
The mass percent of catalyzer each component consists of: HY type molecular sieve 10.8wt%, SAPO-11 molecular sieve 21.6wt%, amorphous aluminum silicide 10.8wt%, pseudo-boehmite 39.7wt%, nickel oxide 7.2wt%, molybdenum oxide 9.9wt%.
The heavy hydrocarbon crack reacting condition is: reaction pressure 10.0Mpa, hydrogen to oil volume ratio 1500, air speed 1.5h
-1, 340 ℃ of temperature of reaction.
Embodiment 8
The ethyl ammonium metatungstate solution is impregnated on the shaping carrier that obtains among the embodiment 3, obtains the catalyzer of tungstenic.All the other preparation process are with embodiment 5.
The mass percent of catalyzer each component consists of: HY type molecular sieve 10.8wt%, SAPO-11 molecular sieve 21.6wt%, amorphous aluminum silicide 10.8wt%, pseudo-boehmite 39.7wt%, nickel oxide 7.2wt%, molybdenum oxide 9.9wt%.
The heavy hydrocarbon crack reacting condition is: reaction pressure 10.0Mpa, hydrogen to oil volume ratio 1500, air speed 1.5h
-1, 340 ℃ of temperature of reaction.
The evaluation result of catalyzer sees Table 1.
The catalytic pyrolysis performance of table 1 catalyzer
| The embodiment numbering | Cleavage rate (%) | Diesel oil selectivity (%) | Isomery selectivity (%) |
| Embodiment 1 embodiment 2 embodiment 3 embodiment 4 embodiment 5 embodiment 6 embodiment 7 embodiment 8 | 83.2 79.4 75.5 77.3 77.8 78.2 80.5 79.2 | 78.7 83.9 89.4 80.2 88.2 87.0 88.0 88.5 | 35.2 42.3 47.2 40.3 47.5 48.0 47.9 46.8 |
Claims (11)
1. hydrocracking catalyst that is used for Tscher-Topsch synthesis of heavy wax, it is characterized in that the each component weight percent is: the HY type molecular sieve of 10.0～24.0wt%, 10.0 the SAPO-11 molecular sieve of～24.0wt%, 3.0 the nickel oxide of～10.0wt%, 0.0 the molybdenum oxide of～15.0wt% or Tungsten oxide 99.999,10.0 the amorphous oxide of～24.0wt%, the pseudo-boehmite of 5.0～65.0wt%.
2, a kind of hydrocracking catalyst that is used for Tscher-Topsch synthesis of heavy wax as claimed in claim 1 is characterized in that described amorphous oxide is amorphous aluminum silicide, amorphous silicon magnesium and modified aluminas.
3, a kind of hydrocracking catalyst that is used for Tscher-Topsch synthesis of heavy wax as claimed in claim 2 is characterized in that described amorphous oxide is an amorphous aluminum silicide.
4, each described preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax of a kind of claim 1-3 is characterized in that comprising the steps:
(1) takes by weighing amorphous oxide, HY and SAPO-11 molecular sieve, behind binding agent pseudo-boehmite mixing, dilute nitric acid solution modulation, kneading and compacting with 5%, drying is 4～6 hours under 100～120 ℃, 4～6 hours postcooling of 500～600 ℃ of roasting temperatures obtain carrier to room temperature in air atmosphere then;
(2) adopt pickling process, the aqueous solution that will contain soluble molybdenum salt or soluble tungsten salt is impregnated on the carrier, evaporating solns is to doing under 100～120 ℃ condition, following dry 4～6 hours at 100～120 ℃ then, 500～600 ℃ of following roastings 4～6 hours, be cooled to room temperature, obtain the intermediates of loaded metal molybdenum or tungsten;
(3) carrier of intermediates that step (2) is obtained or step (1) preparation joins in the nickeliferous soluble salt solution, evaporating solns is to doing under 100～120 ℃ condition, following dry 4～6 hours at 100～120 ℃ then, 500～600 ℃ of following roastings 4～6 hours, be cooled to room temperature, obtain hydrocracking catalyst.
5, the preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax as claimed in claim 4 is characterized in that the described soluble salt that contains molybdenum is a molybdate.
6, the preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax as claimed in claim 5 is characterized in that described molybdate is an ammonium molybdate.
7, the preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax as claimed in claim 4 is characterized in that described nickeliferous soluble salt solution is carbonate or nitrate solution.
8, the preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax as claimed in claim 7 is characterized in that described nickeliferous soluble salt solution is nitrate aqueous solution.
9, the preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax as claimed in claim 4 is characterized in that described soluble tungsten salt is metatungstate or ethyl metatungstate.
10, the preparation method who is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax as claimed in claim 9 is characterized in that described soluble tungsten salt is metatungstate.
11, the described application that is used for the hydrocracking catalyst of Tscher-Topsch synthesis of heavy wax of a kind of claim 9 is characterized in that reaction conditions is: reaction pressure 3.0～10.0Mpa, hydrogen to oil volume ratio 400～1500, volume space velocity 0.5～2.0h
-1, 320～400 ℃ of temperature of reaction.
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| CN102049295B (en) * | 2009-10-27 | 2012-11-21 | 中国石油化工股份有限公司 | Super-deep fraction oil hydrodesulphurization catalyst and preparation method thereof |
| CN103301872A (en) * | 2013-07-11 | 2013-09-18 | 中科合成油内蒙古有限公司 | Non-sulfur catalyst as well as preparation method and application thereof |
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| CN105964294A (en) * | 2016-05-24 | 2016-09-28 | 山东成泰化工有限公司 | Hydrogenation catalyst composition and preparation method thereof |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4842714A (en) * | 1984-11-27 | 1989-06-27 | Uop | Catalytic cracking process using silicoaluminophosphate molecular sieves |
| CN1064862C (en) * | 1994-11-09 | 2001-04-25 | 中国石油化工总公司 | Hydrogen cracking catalyst |
| CN1261542C (en) * | 2003-05-30 | 2006-06-28 | 中国石油化工股份有限公司 | Monox-alumina containnig hydrocracking catalyst |
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2006
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| CN102049295B (en) * | 2009-10-27 | 2012-11-21 | 中国石油化工股份有限公司 | Super-deep fraction oil hydrodesulphurization catalyst and preparation method thereof |
| CN103301872A (en) * | 2013-07-11 | 2013-09-18 | 中科合成油内蒙古有限公司 | Non-sulfur catalyst as well as preparation method and application thereof |
| WO2015172592A1 (en) * | 2014-05-14 | 2015-11-19 | 武汉凯迪工程技术研究总院有限公司 | Catalyst suitable for production of aviation kerosene from biomass fischer-tropsch synthesis oil and preparation method therefor |
| KR101828965B1 (en) * | 2014-05-14 | 2018-02-13 | 우한 카이디 엔지니어링 테크놀로지 리서치 인스티튜트 코오퍼레이션 엘티디. | Catalyst suitable for production of aviation kerosene from biomass fischer-tropsch synthesis oil and preparation method therefor |
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| CN112337506A (en) * | 2020-11-12 | 2021-02-09 | 陕西延长石油（集团）有限责任公司 | Catalyst for Fischer-Tropsch wax hydrogenation conversion and preparation method and application thereof |
| CN112337506B (en) * | 2020-11-12 | 2023-04-07 | 陕西延长石油（集团）有限责任公司 | Catalyst for Fischer-Tropsch wax hydrogenation conversion and preparation method and application thereof |
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