CN107321380A - A kind of loaded catalyst of catalysis for preparing biodiesel oil and the method for preparing biodiesel - Google Patents
A kind of loaded catalyst of catalysis for preparing biodiesel oil and the method for preparing biodiesel Download PDFInfo
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- CN107321380A CN107321380A CN201710535395.9A CN201710535395A CN107321380A CN 107321380 A CN107321380 A CN 107321380A CN 201710535395 A CN201710535395 A CN 201710535395A CN 107321380 A CN107321380 A CN 107321380A
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- catalyst
- biodiesel
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- grease
- zeolite
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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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- 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
- B01J29/405—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 rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a kind of loaded catalyst of new catalysis for preparing biodiesel oil and the preparation method of biodiesel, the catalyst includes carrier, active component and auxiliary agent, the carrier of the loaded catalyst is one or more of combinations in modified molecular sieve or zeolite, active component is one or more of combinations in V, Zr, Mo or W, and auxiliary component is the one or more in F, Cl or P.The preparation method of biodiesel comprises the following steps：Make grease, lower alcohol and the catalyst haptoreaction in tubular reactor, during grease and lower alcohol enter tubular reactor from tubular reactor bottom, reacting coarse product flows out from tubular reactor upper end, and reaction reclaims excessive methanol after terminating, catalyst is separated and recovered, biodiesel oil product is made.Using biodiesel method technological process of the invention simply, and under lower temperature and pressure the yield of biodiesel is improved.
Description
Technical field
The present invention relates to biodiesel catalyst technical field, in particular it relates to which a kind of catalysis for preparing biodiesel oil is negative
Supported catalyst and the method for preparing biodiesel.
Background technology
Biodiesel generally carries out ester exchange reaction using grease and lower alcohol and is made, and has fatty acid ester in reaction product,
Also monoglyceride, two sweet esters, glycerine, and unreacted alcohol and grease.The preparation method of existing biodiesel can be divided into acid and urge
Change method, base catalysis method, enzyme catalysis method and supercritical methanol technology.
Acid catalyzed process prepares biodiesel can be divided into liquid acid catalyzed process and solid acid catalysis method again.Liquid acid (e.g., dense sulphur
Acid, phosphoric acid, hydrochloric acid, nitric acid, toluene sulfonic acide etc.) as conventional catalyst, the characteristics of with high catalytic efficiency, but liquid acid
There is peril of transportation in catalyst, strong to equipment corrosion, post processing separating-purifying is difficult, causes, and limit
Its commercial Application.Compared to liquid acid catalyst, solid acid catalyst catalyst is easily reclaimed, regenerated；Locate after the product of preparation
Reason is simple, and the corrosivity to equipment is small.
The content of the invention
The invention provides the preparation of a kind of loaded catalyst of new catalysis for preparing biodiesel oil and biodiesel
Method, it is simple using the biodiesel method technological process, and improve biology under lower temperature and pressure
The yield of diesel oil.
The invention provides a kind of loaded catalyst of catalysis for preparing biodiesel oil, the catalyst includes carrier, work
Property component and auxiliary agent, the carrier of the loaded catalyst is one or more of combinations in modified molecular sieve or zeolite,
Active component is one or more of combinations in V, Zr, Mo or W, and auxiliary component is the one or more in F, Cl or P.
Present invention also offers a kind of preparation method of biodiesel, comprise the following steps：Make grease, lower alcohol and catalysis
During agent haptoreaction in tubular reactor, grease and lower alcohol enter tubular reactor from tubular reactor bottom, reaction is thick
Product flows out from tubular reactor upper end, and excessive methanol is reclaimed in reaction after terminating, and separates and recovers catalyst, and biodiesel production is made
Product.
The method of the present invention can prepare biodiesel at relatively low temperatures and pressures, it is not necessary to which the grease is carried out
Pre-process (such as pre-esterification processing), simplify the process for preparing biodiesel, and the yield of biodiesel can be improved, greatly improve
Production efficiency.
Embodiment
The embodiment to the present invention is described in detail below.
First purpose of the present invention is to provide a kind of loaded catalyst of catalysis for preparing biodiesel oil.
To achieve the above object, adopt the following technical scheme that：
A kind of loaded catalyst of catalysis for preparing biodiesel oil, the catalyst includes carrier, active component and auxiliary agent,
Characterized in that, the carrier of the loaded catalyst is one or more of combinations in modified molecular sieve or zeolite, it is living
Property component be V, Zr, Mo or W in one or more of combinations, auxiliary component be F, Cl or P in one or more, the work
The consumption of property component in the catalyst is calculated as 10-40wt%, preferably 20-35wt% with oxide, and the auxiliary agent is in the catalyst
Consumption 1-10wt%, preferably 3-8% are calculated as with element；
The method of modifying of molecular sieve or zeolite is molecular sieve or zeolite to be fitted into reaction tube, in a nitrogen atmosphere with 5-
10 DEG C/min speed is warming up under 500-700 DEG C, normal pressure using mass space velocity as 2-5h-1100% vapor is passed through, and continues 2-
5h, then stops being passed through vapor, is passed through nitrogen and is down to room temperature, obtain modified molecular sieve or zeolite.
The molecular sieve is a kind of in ZSM-11, ZSM-22, modenite, erionite or combines, preferably ZSM-22.
The catalyst is prepared using infusion process, and step is as follows：The predecessor of active component is dissolved in deionized water, plus
Enter auxiliary component, obtain mixed solution, impregnated 10-20 hours with modified molecular sieve or zeolite, decompression rotary evaporation removes many
Remaining moisture, in an oven in drying 2~4 at 105~120 DEG C, then in N22~6 are calcined in atmosphere at 400~550 DEG C
Hour, the catalyst is made after cooling.
The predecessor of the active component is water soluble inorganic substance, preferably ammonium vanadate, zirconium nitrate, ammonium molybdate, ammonium tungstate.Help
Agent is into water-soluble substances of the component selections containing F, Cl or P, preferably KF, NaF, KCl, NaCl, H3PO4。
The combination of the combination, more preferably V, Zr and Mo of the preferred metal of active component, in the catalyst V, Zr and Mo
Mol ratio is 1-3: 1: 0.5-1, more preferably 2: 1: 0.5.
It is a further object to provide a kind of preparation method of biodiesel.
The method for the catalysis for preparing biodiesel oil that the present invention is provided comprises the following steps, makes grease, lower alcohol and catalyst
During the haptoreaction in tubular reactor, grease and lower alcohol enter tubular reactor from tubular reactor bottom, the thick production of reaction
Thing flows out from tubular reactor upper end, and excessive methanol is reclaimed in reaction after terminating, and separates and recovers catalyst, and biodiesel production is made
Product, analysis detects its biodiesel production rate.
In the present invention, the grease can be various conventional greases, its main component be fatty acid triglycercide and/or
Aliphatic acid, for example, one kind in kitchen waste grease, acidification oil, vegetable fat, animal fat or microbial grease.
In the present invention, the lower alcohol can be monohydric alcohol of the carbon number between 1-6, it is preferable that the monohydric alcohol is
At least one of methanol, ethanol, propyl alcohol, more preferably methanol and/or ethanol.
The consumption of the catalyst is relative to the grease of 100 parts by weight, and the consumption of catalyst is 0.001-5 parts by weight.More
Under preferable case, relative to the grease of 100 parts by weight, the consumption of catalyst is 0.5-2 parts by weight.
The weight ratio of the grease and lower alcohol can be 1: 0.05-1, preferably 1: 0.1-0.6, more preferably 1: 0.2-
0.6。
The catalytic condition is：Temperature is 150-350 DEG C, and pressure is 0.01-5MPa, and oil plant liquid hourly space velocity (LHSV) is
0.1-20h-1, preferably 0.1-5h-1。
The present invention is described in detail by the following examples.The yield of biodiesel is calculated by following formula：
The yield of biodiesel=(quality of quality/grease of the biodiesel finally obtained) × 100%.
Preparation example 1
ZSM-22 molecular sieves are fitted into reaction tube, 500 DEG C are warming up in a nitrogen atmosphere with 10 DEG C/min speed, often
Pressure is using mass space velocity as 3h-1100% vapor is passed through, and continues 4h, then stops being passed through vapor, is passed through nitrogen and is down to room
Temperature, takes out modified molecular sieve, standby.
Ammonium vanadate is dissolved in deionized water, KF is added, obtains mixed solution, is impregnated 20 hours with modified molecular sieve,
Depressurize rotary evaporation and remove unnecessary moisture, in an oven in drying 4h at 105 DEG C, then in N2Roasted in atmosphere at 400 DEG C
Burn 5 hours, the catalyst is made after cooling, catalyst A is designated as.In catalyst composition, vanadium content in terms of oxide is
30wt%, fluorine counts content as 8wt% using element.
Preparation example 2
According to the method for preparation example 1, difference is that active component presoma is zirconium nitrate, and auxiliary agent is P, is designated as catalyst B,
In catalyst composition, zirconium counts content as 25wt% using oxide, and fluorine counts content as 5wt% using element.
Preparation example 3
According to the method for preparation example 1, difference is that active component presoma is ammonium vanadate, zirconium nitrate, ammonium molybdate, and auxiliary agent is
F, is designated as in catalyst C, catalyst composition, V, Zr and Mo mol ratio are 2: 1: 0.5, and the consumption of active component is in terms of oxide
For 30wt%, fluorine counts content as 4wt% using element.
Preparation example 4
According to the method for preparation example 1, difference is that active component presoma is ammonium tungstate, and auxiliary agent is Cl, is designated as catalyst
In D, catalyst composition, tungsten is calculated as 25wt% with oxide, and Cl counts content as 6wt% using element.
Embodiment 1
Grease, methanol are added in tubular reactor (diameter 10mm, length 800mm) together, grease and methanol quality
Than 1: 0.2, the catalyst A of grease weight 0.6% is added, in 200 DEG C of temperature, pressure 4MPa, liquid hourly space velocity (LHSV) is 1.2h-1Condition
Under, during grease and methanol continuously are squeezed into reactor from the bottom of tubular reactor, reacting coarse product is obtained, reaction is thick
Product mutually obtains biodiesel product, the yield of product through steaming unreacted methanol, standing separation glycerine phase, vacuum distillation ester
For 79.3%.
Embodiment 2
Grease, methanol are added in tubular reactor (diameter 10mm, length 800mm) together, grease and methanol quality
Than 1: 0.4, the catalyst B of grease weight 0.8% is added, in 250 DEG C of temperature, pressure 3MPa, liquid hourly space velocity (LHSV) is 1.5h-1Condition
Under, during grease and methanol continuously are squeezed into reactor from the bottom of tubular reactor, reacting coarse product is obtained, reaction is thick
Product mutually obtains biodiesel product, the yield of product through steaming unreacted methanol, standing separation glycerine phase, vacuum distillation ester
For 81.2%.
Embodiment 3
Grease, methanol are added in tubular reactor (diameter 10mm, length 800mm) together, grease and methanol quality
Than 1: 0.3, the catalyst C of grease weight 0.5% is added, in 230 DEG C of temperature, pressure 3MPa, liquid hourly space velocity (LHSV) is 1.0h-1Condition
Under, during grease and methanol continuously are squeezed into reactor from the bottom of tubular reactor, reacting coarse product is obtained, reaction is thick
Product mutually obtains biodiesel product, the yield of product through steaming unreacted methanol, standing separation glycerine phase, vacuum distillation ester
For 83.5%.
Embodiment 4
Grease, methanol are added in tubular reactor (diameter 10mm, length 800mm) together, grease and methanol quality
Than 1: 0.6, the catalyst D of grease weight 1% is added, in 220 DEG C of temperature, pressure 4MPa, liquid hourly space velocity (LHSV) is 1.5h-1Under the conditions of,
During grease and methanol continuously are squeezed into reactor from the bottom of tubular reactor, reacting coarse product, the thick production of reaction are obtained
Thing mutually obtains biodiesel product through steaming unreacted methanol, standing separation glycerine phase, vacuum distillation ester, and the yield of product is
77.9%.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
Claims (9)
1. a kind of loaded catalyst of catalysis for preparing biodiesel oil, the catalyst includes carrier, active component and auxiliary agent, its
It is characterised by, the carrier of the loaded catalyst is one or more of combinations in modified molecular sieve or zeolite, activity
Component is one or more of combinations in V, Zr, Mo or W, and auxiliary component is the one or more in F, Cl or P, the activity
The consumption of component in the catalyst is calculated as 10-40wt%, preferably 20-35wt% with oxide, and the auxiliary agent is in the catalyst
Consumption is calculated as 1-10wt%, preferably 3-8% with element；
The method of modifying of molecular sieve or zeolite is that molecular sieve or zeolite are fitted into reaction tube, in a nitrogen atmosphere with 5-10 DEG C/
Min speed is warming up under 500-700 DEG C, normal pressure using mass space velocity as 2-5h-1100% vapor is passed through, and continues 2-5h, so
Stop being passed through vapor afterwards, be passed through nitrogen and be down to room temperature, obtain modified molecular sieve or zeolite.
2. loaded catalyst according to claim 1, it is characterised in that the molecular sieve be selected from ZSM-11, ZSM-22,
A kind of or combination, preferably ZSM-22 in modenite, erionite.
3. loaded catalyst according to claim 1, it is characterised in that the catalyst is prepared using infusion process, step
It is rapid as follows：The predecessor of active component is dissolved in deionized water, auxiliary component is added, obtains mixed solution, with modified point
Sub- sieve or zeolite impregnate 10-20 hours, and decompression rotary evaporation removes unnecessary moisture, in an oven in dry at 105-120 DEG C
2-4h, then in N22-6h is calcined in atmosphere at 400-550 DEG C, the catalyst is made after cooling.
4. loaded catalyst according to claim 1, it is characterised in that described active component preferred V, Zr and Mo group
Close, V, Zr and Mo mol ratio are 1-3: 1: 0.5-1.
5. usage right requires the method that the loaded catalyst described in any one of 1-4 prepares biodiesel, comprise the following steps,
Make grease, lower alcohol and the catalyst haptoreaction in tubular reactor, grease and lower alcohol enter from tubular reactor bottom
In tubular reactor, reacting coarse product flows out from tubular reactor upper end, and reaction reclaims excessive methanol after terminating, and separation and recovery is urged
Agent, is made biodiesel oil product.
6. method according to claim 5, it is characterised in that the lower alcohol can be carbon number between 1-6
Monohydric alcohol.
7. method according to claim 5, it is characterised in that oil of the consumption of the catalyst relative to 100 parts by weight
Fat, the consumption of the catalyst is 0.001-5 parts by weight, preferably with respect to the grease of 100 parts by weight, the consumption of the catalyst
For 0.5-2 parts by weight.
8. method according to claim 5, it is characterised in that the weight ratio of the grease and lower alcohol is 1: 0.05-1,
Preferably 1: 0.1-0.6.
9. method according to claim 5, it is characterised in that the catalytic condition is：Temperature is 150-350
DEG C, pressure is 0.01-5MPa, and oil plant liquid hourly space velocity (LHSV) is 0.1-20h-1。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041130A (en) * | 2007-04-12 | 2007-09-26 | 上海三瑞化学有限公司 | Catalysts for solid base for producing biodiesel |
| CN101270300A (en) * | 2008-04-30 | 2008-09-24 | 中国石油天然气股份有限公司 | Hydrogenation deoxidation catalyst for producing biological diesel oil |
| CN102427880A (en) * | 2009-04-01 | 2012-04-25 | Sk新技术株式会社 | Metal phosphorus compound for preparing biodiesel and method for preparing biodiesel using the same |
| CN105296167A (en) * | 2014-07-24 | 2016-02-03 | 中国石油化工股份有限公司 | Method for preparing biodiesel through catalysis |
| EP2995672A1 (en) * | 2013-05-07 | 2016-03-16 | Wuhan Kaidi Engineering Technology Research Institute Co., Ltd. | Method for modifying biomass pyrolysis oil |
-
2017
- 2017-07-03 CN CN201710535395.9A patent/CN107321380B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041130A (en) * | 2007-04-12 | 2007-09-26 | 上海三瑞化学有限公司 | Catalysts for solid base for producing biodiesel |
| CN101270300A (en) * | 2008-04-30 | 2008-09-24 | 中国石油天然气股份有限公司 | Hydrogenation deoxidation catalyst for producing biological diesel oil |
| CN102427880A (en) * | 2009-04-01 | 2012-04-25 | Sk新技术株式会社 | Metal phosphorus compound for preparing biodiesel and method for preparing biodiesel using the same |
| EP2995672A1 (en) * | 2013-05-07 | 2016-03-16 | Wuhan Kaidi Engineering Technology Research Institute Co., Ltd. | Method for modifying biomass pyrolysis oil |
| CN105296167A (en) * | 2014-07-24 | 2016-02-03 | 中国石油化工股份有限公司 | Method for preparing biodiesel through catalysis |
Non-Patent Citations (2)
| Title |
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| 项寿鹤等: "HZSM-20沸石分子筛的水蒸汽改性", 《催化学报》 * |
| 高滋等: "《沸石催化与分离技术》", 30 November 1999 * |
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