CN114250080B - Method for preparing hydrocarbon-rich bio-fuel oil by catalyzing grease deoxidization - Google Patents
Method for preparing hydrocarbon-rich bio-fuel oil by catalyzing grease deoxidization Download PDFInfo
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- CN114250080B CN114250080B CN202111677458.7A CN202111677458A CN114250080B CN 114250080 B CN114250080 B CN 114250080B CN 202111677458 A CN202111677458 A CN 202111677458A CN 114250080 B CN114250080 B CN 114250080B
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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
- C10G3/45—Catalytic treatment characterised by the catalyst used containing iron group metals or compounds thereof
- C10G3/46—Catalytic treatment characterised by the catalyst used containing iron group metals or compounds thereof in combination with chromium, molybdenum, tungsten metals or compounds thereof
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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
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/48—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively 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
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
-
- 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
Abstract
The invention discloses a method for preparing hydrocarbon-rich biofuel by catalyzing grease deoxidation, belonging to the technical field of biomass energy pretreatment. The method is to prepare hydrocarbon-rich biofuel by catalyzing grease raw material deoxidation by using a supported nickel molybdenum rhenium trimetallic catalyst; the mass ratio of the grease to the catalyst is 1:1-100:1, the reaction temperature is 180-350 ℃, the hydrogen pressure is 0.5-10MPa, and the reaction time is 1.0-8.0h. The catalyst does not need to be vulcanized, so that the problem of product pollution caused by sulfur leaching is avoided. The prepared catalyst mainly removes oxygen atoms in grease in the form of water molecules, avoids carbon atom loss and improves the yield of the bio-fuel oil.
Description
Technical Field
The invention belongs to the technical field of biomass energy pretreatment, and particularly relates to a method for preparing hydrocarbon-rich biofuel by catalyzing grease deoxidation.
Background
As the global demand for traditional fossil fuels increases, there is an increasing decrease in fossil energy. On the other hand, the combustion of conventional fossil fuels results in the emission of a large amount of greenhouse gases and toxic gas compounds, which not only causes global warming but also causes serious pollution to the environment. The production of liquid green biofuel from renewable and low cost fats (with fatty acid glycerides and free fatty acids as the main components) is the most attractive option. At present, the catalyst commonly used for preparing the hydrocarbon-rich raw fuel oil by catalyzing grease is mainly metal sulfide (such as NiMoS 4 And CoMoS 4 Etc.) and noble metal catalysts (e.g., gamma-Al 2 O 3 Supported noble metals Pd, pt, ir, etc.). However, the development of noble metal catalysts is severely restricted due to the high price of the catalysts, the severe reaction conditions of metal sulfides, the leaching of toxic element sulfur in the reaction process and other problems. In addition, the catalyst often causes decarboxylation and decarbonylation reaction of grease in the process of catalyzing grease deoxidation, thereby causing partial loss of carbon atoms and reducing the yield of the hydrocarbon-rich biofuel.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problem to be solved by the invention is to provide a method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxidation, which uses a NiMoRe/H-ZSM-5 catalyst with low cost, and the catalyst does not need to be vulcanized, so that the problems that the noble metal catalyst has high price and the sulfur element is leached out in the grease hydrodeoxygenation process to cause pollution to products are solved.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for preparing hydrocarbon-rich biofuel by catalyzing grease deoxidization utilizes a supported nickel-molybdenum-rhenium trimetallic catalyst to catalyze grease raw material deoxidization to prepare hydrocarbon-rich biofuel; the mass ratio of the grease to the catalyst is 1:1-100:1, the reaction temperature is 180-350 ℃, the hydrogen pressure is 0.5-10MPa, and the reaction time is 1.0-8.0h.
The method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxidation is characterized in that a supported nickel-molybdenum-rhenium trimetallic catalyst is prepared by adopting an impregnation method.
According to the method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxygenation, the loading amount of fixed metal nickel in the supported nickel-molybdenum-rhenium three-metal catalyst is 10wt%, the loading amount of rhenium is 2wt%, and the molar ratio of the supported metal nickel to molybdenum is 0.1:1-6:1.
According to the method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing the grease to deoxidize, the mass ratio of the grease to the catalyst is 5:1-10:1, the reaction temperature is 200-260 ℃, the hydrogen pressure is 4.0-5.0MPa, and the reaction time is 3.0-8.0h.
According to the method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxygenation, the loading amount of fixed metal nickel in the supported nickel-molybdenum-rhenium three-metal catalyst is 10wt%, the loading amount of rhenium is 2wt%, and the molar ratio of the supported metal nickel to molybdenum is 0.5:1-2:1.
According to the method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxygenation, the supported nickel-molybdenum-rhenium trimetallic catalyst is NiMoRe/H-ZSM-5, and Si/Al=25 in the carrier H-ZSM-5.
The method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxidization comprises the following steps of:
(1) Ni (NO) 3 ) 2 ·6H 2 O、(NH 4 ) 6 Mo 7 O 24 ·4H 2 O and NH 4 ReO 4 Dissolving in distilled water, and stirring at 60deg.C; adding the H-ZSM-5 carrier into the salt solution, stirring for 3.0H, and evaporating the solvent to obtain a catalyst precursor;
(2) Drying the catalyst precursor for 12 hours at the temperature of 100 ℃, and roasting the dried solid for 5.0 hours at the temperature of 400 ℃ to obtain the catalyst NiMoRe/H-ZSM-5.
The method for preparing the hydrocarbon-rich biological fuel oil by catalyzing grease deoxidation comprises the following steps:
(1) Adding an oil raw material and a supported nickel-molybdenum-rhenium trimetallic catalyst into a reaction vessel, purging the reaction vessel by using hydrogen to remove internal air, pressurizing the reaction vessel, heating to a reaction temperature, and starting the reaction;
(2) After the reaction is finished, separating the reaction liquid to obtain diesel chain alkane and a catalyst.
According to the method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxidization, the catalyst is reduced for 3.0h under the pure hydrogen condition at 500 ℃ before being used.
According to the method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxygenation, the grease raw material is soybean oil.
The beneficial effects are that: compared with the prior art, the invention has the advantages that:
(1) The catalyst does not need to be vulcanized, so that the problem of product pollution caused by sulfur leaching is avoided.
(2) High catalytic activity, mild reaction condition, 180-350 deg.c and 0.5-10MPa H pressure 2 The aim of converting grease into the hydrocarbon-rich biological fuel oil can be fulfilled within the range.
(3) The prepared catalyst mainly removes oxygen atoms in grease in the form of water molecules, avoids carbon atom loss and improves the yield of the bio-fuel oil.
(4) The catalyst has low preparation cost and no addition of any elements harmful to the environment.
Drawings
FIG. 1 is a gas chromatogram of the liquid product of example 2.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof. The results of calculation of alkane yield are shown below:
example 1
Preparation of catalyst NiMoRe/H-ZSM-5:
nickel nitrate hexahydrate (Ni (NO) 3 ) 2 ·6H 2 O), ammonium molybdate ((NH) 4 ) 6 Mo 7 O 24 ·4H 2 O) and ammonium perrhenate (NH) 4 ReO 4 ) H-ZSM-5 (Si/Al=25) was used as a carrier for the desired inorganic salt. The specific synthesis steps are as follows:
(1) Ni (NO) 3 ) 2 ·6H 2 O、(NH 4 ) 6 Mo 7 O 24 ·4H 2 O and NH 4 ReO 4 Dissolving in distilled water, and stirring at 60deg.C. Next, H-ZSM-5 carrier was added to the above salt solution at 60 ℃. After stirring at 60 ℃ for about 3.0 hours, the solvent was evaporated to obtain a catalyst precursor; wherein the loading of Ni is 10wt%, the loading of Re is 2wt%, and the molar ratio of Ni to Mo is 1:1;
(2) Drying the obtained solid at 100 ℃ for 12 hours, and roasting the dried solid at 400 ℃ for 5.0 hours to obtain a catalyst NiMoRe/H-ZSM-5;
(3) The catalyst was reduced at 500 ℃ under pure hydrogen for 3.0h and applied to the preparation of hydrocarbon-rich bio-fuels by catalytic grease deoxygenation of examples 2-9.
Example 2
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 3g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 6.0MPa. The heating switch is turned on, the temperature is raised to 210 ℃, and the temperature is kept for 8.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 83wt%.
Example 3
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 3g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 6.0MPa. The heating switch is turned on, the temperature is raised to 200 ℃, and the temperature is kept for 5.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 72wt%.
Example 4
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 3g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 5.0MPa. The heating switch is turned on, the temperature is raised to 250 ℃, and the temperature is kept for 6.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 84wt%.
Example 5
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 3g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 5.0MPa. The heating switch is turned on, the temperature is raised to 300 ℃, and the temperature is kept for 3.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 83wt%.
Example 6
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 3g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 6.0MPa. The heating switch is turned on, the temperature is raised to 210 ℃, and the temperature is kept for 5.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 76wt%.
Example 7
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 3g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 5.0MPa. The heating switch is turned on, the temperature is raised to 230 ℃, and the temperature is kept for 6.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 80wt%.
Example 8
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 1g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 6.0MPa. The heating switch is turned on, the temperature is raised to 250 ℃, and the temperature is kept for 8.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 75wt%.
Example 9
A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing soybean oil deoxidization specifically comprises the following steps:
10g of soybean oil and 2g of the catalyst prepared in example 1 were added to a 50mL reaction vessel, and the stirring rate was set at 1000r/min. The reaction vessel was purged with hydrogen 3 times to remove internal air, and then, the reaction vessel was pressurized to 5.0MPa. The heating switch is turned on, the temperature is raised to 300 ℃, and the temperature is kept for 5.0h. After the reaction vessel cooled to room temperature, the liquid product after the reaction was analyzed and the catalyst was recovered. The yield of alkane was about 84wt%.
Claims (4)
1. A method for preparing hydrocarbon-rich biofuel by catalyzing grease deoxidation is characterized in that a supported nickel-molybdenum-rhenium trimetallic catalyst is utilized to catalyze grease raw material deoxidation to prepare hydrocarbon-rich biofuel; the supported nickel molybdenum rhenium trimetallic catalyst is NiMoRe/H-ZSM-5, and Si/Al=25 in the carrier H-ZSM-5;
the preparation method of the catalyst NiMoRe/H-ZSM-5 comprises the following steps:
(1) Ni (NO) 3 ) 2 •6H 2 O、(NH 4 )6Mo 7 O 24 •4H 2 O and NH 4 ReO 4 Dissolving in distilled water, and stirring at 60deg.C; adding the H-ZSM-5 carrier into the salt solution, stirring for 3.0 and H, and evaporating the solvent to obtain a catalyst precursor;
(2) Drying the catalyst precursor for 12 hours at 100 ℃, and roasting the dried solid at 400 ℃ for 5.0. 5.0H to obtain a catalyst NiMoRe/H-ZSM-5;
the loading of the fixed metal nickel in the supported nickel-molybdenum-rhenium trimetallic catalyst is 10wt%, the loading of rhenium is 2wt%, and the molar ratio of the supported metal nickel to molybdenum is 0.1:1-6:1;
the mass ratio of the oil raw material to the catalyst is 5:1-10:1, the reaction temperature is 200-260 ℃, the hydrogen pressure is 4.0-5.0MPa, and the reaction time is 3.0-8.0 h; the catalyst was reduced to 3.0. 3.0h under pure hydrogen at 500 ℃ without sulfiding.
2. The method for preparing the hydrocarbon-rich biofuel from the catalytic grease according to claim 1 is characterized in that the loading of the fixed metallic nickel in the supported nickel-molybdenum-rhenium trimetallic catalyst is 10wt percent, the loading of rhenium is 2 percent by weight, and the molar ratio of the supported metallic nickel to molybdenum is 0.5:1-2:1.
3. The method for preparing the hydrocarbon-rich bio-fuel oil by catalyzing grease deoxygenation according to claim 1 is characterized by comprising the following steps:
(1) Adding an oil raw material and a supported nickel-molybdenum-rhenium trimetallic catalyst into a reaction vessel, purging the reaction vessel by using hydrogen to remove internal air, pressurizing the reaction vessel, heating to a reaction temperature, and starting the reaction;
(2) After the reaction is finished, separating the reaction liquid to obtain diesel chain alkane and a catalyst.
4. A method for preparing hydrocarbon-rich bio-fuel oil by catalyzing grease deoxygenation according to claim 1 or 3, wherein the grease raw material is soybean oil.
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| US20150057475A1 (en) * | 2013-08-23 | 2015-02-26 | Battelle Memorial Institute | Bi-functional catalyst and processes for conversion of biomass to fuel-range hydrocarbons |
| CN105441108B (en) * | 2014-08-20 | 2017-08-25 | 中国科学院青岛生物能源与过程研究所 | A kind of method that triglycerides hydrogenation deoxidation prepares diesel component |
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