CN106540743A - A kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof - Google Patents
A kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof Download PDFInfo
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- CN106540743A CN106540743A CN201610936427.1A CN201610936427A CN106540743A CN 106540743 A CN106540743 A CN 106540743A CN 201610936427 A CN201610936427 A CN 201610936427A CN 106540743 A CN106540743 A CN 106540743A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
- B01J29/045—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/42—Catalytic treatment
- C10G3/44—Catalytic treatment characterised by the catalyst used
- C10G3/48—Catalytic treatment characterised by the catalyst used further characterised by the catalyst support
- C10G3/49—Catalytic treatment characterised by the catalyst used further characterised by the catalyst support containing crystalline aluminosilicates, e.g. molecular sieves
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/50—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids in the presence of hydrogen, hydrogen donors or hydrogen generating compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/54—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids characterised by the catalytic bed
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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- Materials Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof, method comprises the steps：1）Nickel salt and molybdenum salt are impregnated into into 41 molecular sieve carriers of Al MCM simultaneously, catalyst precursor are obtained through air roasting, then through hydrogen reducing, are obtained catalyst xNiyMo/Al MCM 41（X, y are respectively the mass fraction of Ni, Mo, x=0 ~ 0.2；y=0~0.2）, its active component mass fraction total amount is 5%～30%.2）The catalyst is loaded into Solid Bed, while being passed through nitrogen, hydrogen and jatropha oil, is reacted under 330 ~ 370 DEG C of reaction temperature.3）Product is cooled down, and is removed water and is obtained bio-aviation fuel, and outward appearance is as clear as crystal liquid.The features such as catalyst obtained by the present invention has cheap and easy to get, catalysis activity is high, for promoting, Aviation Fuel development and energy sustainable development are significant.In catalyst activity evaluation experimental, jatropha oil hydrogenation deoxidation cracking isomerisation conversion is 100%, and Aviation Fuel yield is 21.5%～73.9%.
Description
Technical field
The present invention relates to a kind of catalyst for preparing biological Aviation Fuel and preparation method thereof.It is mainly used in barbados nut
Oily hydrogenation deoxidation cracking isomerization is prepared in biological Aviation Fuel technique.The invention belongs to catalysis technical field.
Background technology
Aviation Fuel is only second to one of transport fuel of motor petrol and diesel oil as demand, is that a national development must
Indispensable strategic goods and materials.Aviation Fuel is by straight-run, is hydrocracked and component and the necessary addition such as hydrofinishing
A kind of transparency liquid that agent reconciles.Mainly it is made up of the hydrocarbon compound of different fractions, typically by the straight chain of 8～16 carbon
Saturated alkane, isoparaffin, cycloalkane and aromatic hydrocarbons composition.At present due to the day by day exhaustion and energy-saving and emission-reduction measure of fossil fuel
Implement, when realizing improving aero-engine fuel efficiency, increasing researcher is devoted to finding cleaning, environmental protection, can hold
On the bio-fuel of supervention exhibition.
Biomass energy is a kind of biodegradable, reproducible clear energy sources, and its combustibility is similar to petrifaction diesel,
But the pollutant discharge amount of its combustion tail gas is much smaller than petrifaction diesel.Petrifaction diesel is substituted by using biodiesel to be conducive to
Energy-saving and emission-reduction are realized, is had significant practical applications to building a resource-conserving and environment-friendly society.
Leprosy fruit tree is a kind of of many uses, and with drought-resistant ability, growth is rapid, and fruit oil content is high, is suitable as making a living
The raw material of the material energy.And leprosy fruit tree does not account for arable land, cultivation low cost is cultivated, comprehensive development and utilization potential is high.With life
The development of biomass fuel research, jatropha oil become and prepare one of desirable feedstock of bio-fuel.
Provide in patent CN103920528 A a kind of for grease（Comprising grease model compound, grease and its spread out
It is biological）The cracking isomerization of one step hydrogenation deoxidation prepares catalyst of Aviation Fuel and preparation method thereof, it is indicated that grease is through Pd/
（beta-Al2O3）One step catalytic hydrogenation reaction of catalyst is converted into Aviation Fuel key component hydro carbons, reduces hydrogen consumption and energy consumption.
105567284 A of patent CN provides a kind of method for preparing long chain alkane and aromatic hydrocarbons simultaneously as raw material with microalgae oil, microalgae oil
Hydrolyze with water Hybrid Heating, the C that Jing process is obtained10～C22, there is decarboxylation aromatisation under Pd/C catalyst actions anti-in aliphatic acid
Should, the important component long chain alkane and aromatic hydrocarbons of aviation kerosine are obtained, while the hydrogen consumption for preparing aviation kerosine can be greatly lowered.
104448337 B of patent CN provides a kind of method that lignocellulosic efficient catalytic generates Aviation Fuel, will use ionic liquid
The lignin hydrogenation deoxidation that body-aqueous systems are extracted from lignocellulosic is converted into alkane, and then obtains Aviation Fuel,
Wherein used catalyst is Pd/C catalyst.102994138 B of patent CN provides a kind of with waste oil as raw material preparation aviation
The method of kerosene, is fractionated after filter residue, desalination, dehydration, desolventing technology, again in Pd/Al2O3With ammonium formate under catalyst action
In circulating microwave reaction device interior circulation 3～5 times, Jing after ethyl acetate extraction desalination, dehydration, be fractionated and obtain biological aviation coal
Oil.But above-mentioned several use noble metal catalyst, the preparation cost of catalyst is of a relatively high, extensive utilization industrially
It is restricted.Report in PtPd/Al in Energy Fuels2012,26,2394-23992O3And NiMoP/Al2O3Catalyst
On, T=350 °C, LHSV=2 h−1, P=3MPa, H2Jatropha oil is hydrogenated with the conditions of the mL/mL of/oil=600
Prepare the research of bio-fuel-oil.NiMo/B is described in Catalysis Today 164 (2011) 533-5372O3-Al2O3Urge
Agent can obtain the bio-fuel-oil of higher yields at 350 DEG C to waste oil catalytic hydrogenation under the conditions of 5Mpa.Green Chem.,
NiMoLa/Al is described in 2012,14,2499-25052O3Catalyst adds to jatropha oil under the conditions of 3.5Mpa at 370 DEG C
Hydrogen process obtains the alkane that main component is C15～C18.NiMo catalyst is distinguished in Fuel 159 (2015) 430-435
It is carried on Al2O3With on two kinds of different carriers of SAPO-11 at 380 °C, 3Mpa, H2Flow velocity is to have carried out catalysis to add under 400ml/min
Hydrogen process, obtains the product of different paraffin selectivities to the activity experiment of jatropha oil（C is consisted of mainly8～C18Alkane）.
Research of the jatropha oil Hydrogenation for bio-fuel-oil is all referred in above-mentioned several, the fuel oil primary product of gained is long chain alkane,
The fuel oil calorific value for obtaining has no report.But bio-aviation fuel also needs to the components such as a small amount of aromatic hydrocarbons, alkene and branched paraffin.
This several reaction condition is relatively harsh simultaneously, and hydrogen consumption or energy consumption are all higher.
The content of the invention
Based on above content, the present invention devises a kind of jatropha oil hydrogenation deoxidation that is used for and cracks isomerization to prepare biology
A kind of cheap metal catalyst of Aviation Fuel, there is provided catalyst that can prepare alternative Aviation Fuel and preparation method thereof.
The present invention is obtained the catalyst of Aviation Fuel as target through one-step method to jatropha oil to design.
In the present invention, biological Aviation Fuel is C6～C18Liquefied hydrocarbon, comprising positive structure and isoparaffin, alkene, cycloalkane
And aromatic hydrocarbons.The biological Aviation Fuel has higher calorific value, low viscosity, good combustibility, can improve the effect of fuel oil
Rate the effectively discharge of reduction carbon dioxide.
To realize object above, technical scheme below is this invention takes：
The cracking isomerization of jatropha oil hydrogenation deoxidation prepares the catalyst of biological Aviation Fuel, by active metal Ni, Mo or Ni and
Mo, and carrier Al-MCM-41 compositions.It is expressed as xNiyMo/Al-MCM-41（The mass fraction of x, y respectively Ni, Mo, x=0 ~
0.2；y=0~0.2）.Active metal is carried on Al-MCM-41 carriers by conventional impregnation method.
The molecular sieve-4 A l-MCM-41 preparation methods are as follows：
The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine water nitre are added
Sour aluminium is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.Use dilute nitre
Acid-conditioning solution pH=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Program liter after suction filtration, drying
Temperature is obtained carrier Al-MCM-41 to 540 DEG C of roastings.
The concrete preparation method of above-mentioned catalyst is as follows：
By the metal salt solution for preparing（Metal quality fraction is 5%～30%）It is added in carrier Al-MCM-41, using routine
Infusion process, oil bath are evaporated, after 500 DEG C ~ 800 DEG C roastings in Muffle furnace, temperature programmed reduction（Reduction temperature 300 DEG C～900
℃）Prepare catalyst series.
In above-mentioned catalyst preparation process, slaine used is six water nickel nitrates, ammonium molybdate tetrahydrate.
Catalyst activity of the present invention is completed on fixed bed evaluating apparatus, is comprised the following steps that：
Proper catalyst is loaded on into reaction tube flat-temperature zone, catalyst is scatter by ceramic ring, 330 DEG C ~ 370 DEG C of reaction temperature, pressure 0
~ 3Mp, is passed through hydrogen/nitrogen ratio for (5/1 ~ 1/5), 0.025 ~ 0. 05ml/min of feedstock oil jatropha oil inlet amount.
After reaction terminates, step-down cooling is analyzed with GC-MS and GC respectively to product liquid and gaseous product.
The present invention is loaded to active component Ni, Mo or Ni and Mo on Al-MCM-41 carriers by infusion process, is prepared
The cracking isomerization of jatropha oil hydrogenation deoxidation prepares the catalyst of biological Aviation Fuel.The present invention prepares catalyst method simply,
Catalysis activity is high, and catalyst regenerative operation is simple.The biological Aviation Fuel obtained by catalyst preparation of the present invention has higher
Calorific value, low viscosity, can improve fuel oil efficiency and effectively reduce carbon dioxide discharge.In catalyst activity evaluation
In, jatropha oil hydrogenation deoxidation cracking isomerisation conversion is 100%, and biological Aviation Fuel yield is 21.5%～73.8%, is obtained
To bio-aviation fuel calorific value reached 44.8 MJ/kg.
Compared with prior art, the invention has the beneficial effects as follows：
（1）Metal active constituent used by catalyst is prepared for cheap metal, preparation method is simple, reduces being prepared into for catalyst
This, with good prospects for commercial application.
（2）Catalyst prepared by the present invention is obtained biological Aviation Fuel through one-step method to jatropha oil, is tool
There is the multifunction catalyst of hydrogenation, deoxidation, cracking, isomerization.Products therefrom need not pass through complicated separating step can be straight
Connect and obtain biological Aviation Fuel, shorten the liquefaction cycle, reduce energy consumption, to a great extent reduce production Aviation Fuel into
This.
（3）Raw material jatropha oil used herein derives from manioca, and manioca growth is rapid, fruit oil content
Height, is highly suitable as the raw material of biomass energy.And manioca does not account for arable land, cultivation low cost, comprehensive exploitation profit are cultivated
It is high with potential.
Specific embodiment
The present invention is will be further illustrated in the following example, but is not limited the invention.
The preparation of 1. 20%Ni/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）The aqueous solution（The mass fraction of Ni is Al-MCM-41
The 20% of carrier quality fraction）It is added in carrier Al-MCM-41, it is using conventional impregnation method, first clear in KQ-300E type ultrasonic waves
Wash ultrasound 1h in device, steeped overnight, oil bath drying, temperature programming to 600 DEG C, reductase 12 h.
Prepared catalyst n i mass fractions are 20% that 16.7%, Al-MCM-41 molecular sieve quality fractions are 83.3%
Ni/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, the charging of feedstock oil jatropha oil
Amount 0.025ml/min, reacts 5h.
The preparation of 2. 20%Ni/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）The aqueous solution（The mass fraction of Ni is Al-MCM-41
The 20% of carrier quality fraction）It is added in carrier Al-MCM-41, it is using conventional impregnation method, first clear in KQ-300E type ultrasonic waves
Wash ultrasound 1h in device, steeped overnight, oil bath drying, temperature programming to 800 DEG C, reductase 12 h.
Prepared catalyst n i mass fractions are 20% that 16.7%, Al-MCM-41 molecular sieve quality fractions are 83.3%
Ni/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, the charging of feedstock oil jatropha oil
Amount 0.025ml/min, reacts 5h.
The preparation of 3.20% Mo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take the ammonium molybdate tetrahydrate of amount of calculation（(NH4)6Mo2O24·4H2O）The aqueous solution（The mass fraction of Mo is Al-MCM-
The 20% of 41 carrier quality fractions）It is added in carrier Al-MCM-41, using conventional impregnation method, first in KQ-300E type ultrasonic waves
Ultrasound 1h in washer, steeped overnight, oil bath drying, temperature programming to 600 DEG C, reductase 12 h.
Prepared catalyst Mo mass fractions are 20% that 16.7%, Al-MCM-41 molecular sieve quality fractions are 83.3%
Mo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, the charging of feedstock oil jatropha oil
Amount 0.025ml/min, reacts 5h.
The preparation of 4. 20%Mo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take the ammonium molybdate tetrahydrate of amount of calculation（(NH4)6Mo2O24·4H2O）The aqueous solution（The mass fraction of Mo is Al-MCM-
The 20% of 41 carrier quality fractions）It is added in carrier Al-MCM-41, using conventional impregnation method, first in KQ-300E type ultrasonic waves
Ultrasound 1h in washer, steeped overnight, oil bath drying, temperature programming to 800 DEG C, reductase 12 h.
The mass fraction of prepared catalyst Mo is 83.3% for 16.7%, Al-MCM-41 molecular sieve quality fractions
20%Mo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, and feedstock oil jatropha oil enters
Doses 0.025ml/min, reacts 5h.
The preparation of 5. 2.5%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 2.5% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
600 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 4.8%, Al-MCM-41 molecular sieve qualities fraction be 95.2%
2.5%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil leprosy
Oily inlet amount 0.025ml/min of fruit, reacts 5h.
The preparation of 6. 2.5%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 2.5% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
800 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 4.8%, Al-MCM-41 molecular sieve qualities fraction be 95.2%
2.5%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil leprosy
Oily inlet amount 0.025ml/min of fruit, reacts 5h.
The preparation of 7. 5%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 5% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41, adopts
With conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
600 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 9.2%, Al-MCM-41 molecular sieve qualities fraction be 90.8%
5%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 8. 5%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 5% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41, adopts
With conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
800 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 9.2%, Al-MCM-41 molecular sieve qualities fraction be 90.8%
5%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 9. 10%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 10% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
300 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 18.4%, Al-MCM-41 molecular sieve qualities fraction be 81.6%
10%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 10. 10%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 10% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
400 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 18.4%, Al-MCM-41 molecular sieve qualities fraction be 81.6%
10%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 11. 10%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 10% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
600 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 18.4%, Al-MCM-41 molecular sieve qualities fraction be 81.6%
10%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 12. 10%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 10% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
700 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 18.4%, Al-MCM-41 molecular sieve qualities fraction be 81.6%
10%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 13. 10%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 10% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
800 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 18.4%, Al-MCM-41 molecular sieve qualities fraction be 81.6%
10%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 14. 10%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 10% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
900 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 18.4%, Al-MCM-41 molecular sieve qualities fraction be 81.6%
10%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 15. 15%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 15% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
600 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 27.6%, Al-MCM-41 molecular sieve qualities fraction be 72.4%
15%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
The preparation of 16. 15%NiMo/ Al-MCM-41 catalyst of embodiment
（1）The cetyl trimethylammonium bromide (CTAB) and NaOH of amount of calculation are dissolved in deionized water, nine are added
Water aluminum nitrate is in solution to being completely dissolved. and then appropriate tetraethyl orthosilicate (TEOS) is slowly added dropwise, persistently stir 2 h.With
Dust technology adjusts pH value of solution=5.5.Stand after being stirred for 3 h.Filter, be washed with deionized to neutrality.Journey after suction filtration, drying
Sequence is warming up to 540 DEG C of roastings, and carrier Al-MCM-41 is obtained.
（2）Take six water nickel nitrates of amount of calculation（Ni(NO3)2·6H2O）And ammonium molybdate tetrahydrate（(NH4)6Mo2O24·4H2O）
The aqueous solution（The mass fraction of Ni, Mo is the 15% of Al-MCM-41 carrier quality fractions）It is added in carrier Al-MCM-41,
Using conventional impregnation method, first the ultrasound 1h in KQ-300E type ultrasonic cleaners, steeped overnight, oil bath drying, temperature programming is extremely
800 DEG C, reductase 12 h.
Prepared catalyst n i, Mo mass fraction and for 27.6%, Al-MCM-41 molecular sieve qualities fraction be 72.4%
15%NiMo/ Al-MCM-41 catalyst, at 360 DEG C, pressure 3Mp, H2、N2Flow velocity is 100ml/min, feedstock oil barbados nut
Oily inlet amount 0.025ml/min, reacts 5h.
Finally, it should be noted that listed above is only specific embodiment of the invention.The invention is not restricted to above reality
Example is applied, there can also be many variations, those skilled in the art can directly derived all changes from present disclosure
Shape, is considered as the scope of protection of the invention.
The evaluation result row of prepared hydrogenation deoxidation cracking isomerization catalyst in above-described embodiment 1～4,9～11,13～14
In shown in table 1.
Table 1
In table, conversion ratio computing formula is：
C=［ M (T0)-M (n)/M (T0) * 100%, wherein M (T0) the quality percentage before and after feedstock oil reaction is respectively with M (n)
Number.
Biological Aviation Fuel yield computing formula is：
Y=ΣM(i)/ M(T0) * 100%, wherein Σ M (i) is C6～C18Constituent mass fraction sum.
N-alkane selectivity computing formula be：
S（a）=Σ M (a)/［ M (T0)-M (n) * 100%, wherein Σ M (a) is n-alkane mass percent sum.
Isoparaffin selectivity computing formula is：
S（b）=Σ M (b)/［ M (T0)-M (n) * 100%, wherein Σ M (b) is isoparaffin mass percent sum.
Cycloalkanes hydrocarbon-selective computing formula is：
S（c）=Σ M (c)/［ M (T0)-M (n) * 100%, wherein Σ M (c) is cycloalkane mass percent sum.
Arenes selectivity computing formula is：
S（d）=Σ M (d)/［ M (T0)-M (n) * 100%, wherein Σ M (d) is aromatics quality percentage sum.
Other components computing formula is：
S（e）=Σ M (e)/［ M (T0)-M (n) * 100%, wherein Σ M (e) is other components mass percent sum.
Claims (9)
1. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof, it is characterised in that concrete to wrap
Include following steps：
（1）The catalyst adopts the Al-MCM-41 molecular sieves for preparing gained for carrier, while carrying transition metal nickel salt, molybdenum salt
Mixture is formed, then conventional steeped overnight, 80 DEG C ~ 120 DEG C drying are calcined at 500 DEG C ~ 800 DEG C, obtain metal active constituent
Mass fraction total amount is 5%～30% catalyst precursor；
（2）By step（1）Obtained presoma is proceeded in tube furnace, adopt heating rate for 2 DEG C ~ 10 DEG C/min temperature programming
Method of reducing, in 10% ~ 100% hydrogen atmosphere, reduction temperature is 300 DEG C ~ 900 DEG C reductase 12 ~ 6 hour, obtains xNiyMo/
Al-MCM-41 catalyst（X, y are respectively the mass fraction of Ni, Mo, x=0 ~ 0.2；y=0~0.2）；
（3）By step（2）The catalyst of gained loads fixed bed reactors, is passed through hydrogen/nitrogen ratio for (5/1 ~ 1/5), leprosy
The flow velocity of fruit oil is 0.025 ~ 0.05ml/min, heats to, and the product for obtaining is
Obtained bio-aviation fuel.
2. as claimed in claim 1 a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof, its
It is characterised by, the catalyst can be obtained biological Aviation Fuel through one-step method to jatropha oil.
3. as claimed in claim 1 or 2 a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof,
Characterized in that, the product liquid of gained catalytic hydrogenation is C6～C18Hydro carbons, with positive structure and isoparaffin, alkene, aromatic hydrocarbons and
Based on cycloalkane, product liquid outward appearance is as clear as crystal.
4. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof described in claim 1, which is special
Levy and be, the step（1）The specific surface of middle carrier is in 500～930 m2/g。
5. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof described in claim 1, which is special
Levy and be, the step（2）The aperture of middle catalyst is in 5～15nm.
6. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof described in claim 1, which is special
Levy and be, the step（2）The specific surface of middle catalyst is in 60～500 m2/g。
7. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof described in claim 1, which is special
Levy and be, the step（3）In fixed bed reactors adopt continuously hydrogen adding flow reactor.
8. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof described in claim 1, which is special
Levy and be, the step（3）Middle jatropha oil is 1～2 with the mass ratio of catalyst.
9. a kind of catalyst that biological Aviation Fuel is prepared for jatropha oil and preparation method thereof described in claim 1, which is special
Levy and be, the step（3）Middle jatropha oil is 4～8 with the mass ratio of catalyst.
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