CN103614155B - A kind of algae oil produces the preparation method of HC fuel - Google Patents
A kind of algae oil produces the preparation method of HC fuel Download PDFInfo
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- CN103614155B CN103614155B CN201310413871.1A CN201310413871A CN103614155B CN 103614155 B CN103614155 B CN 103614155B CN 201310413871 A CN201310413871 A CN 201310413871A CN 103614155 B CN103614155 B CN 103614155B
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- 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 kind of algae oil and produce the preparation method of HC fuel, the method comprises the following steps: in nitrogen atmosphere, by oil compounds by being pumped into, equipped with the tubular reactor of supported molybdenum catalyst carries out catalytic decarboxylation reaction, obtaining HC fuel；The reaction atmosphere of described decarboxylation deoxidation reaction is nitrogen, and reaction pressure is normal pressure, and reaction temperature is 300 360 DEG C, and the response time is 1.5 3.0h, and feed rate is 0.03 0.30g/(cm2Min)；Wherein said supported molybdenum catalyst is with molybdenum as active metal, with activated carbon as catalyst carrier.Compared with prior art, owing to the present invention uses the supported molybdenum catalyst with activated carbon as carrier, its catalysis activity is high, and reaction condition is gentle (reaction need not hydrogen, and can carry out at ambient pressure), and the conversion ratio of raw material and DNA vaccine and liquid hydrocarbon productivity are higher.
Description
Technical field
The present invention relates to biomass energy preparing technical field, a kind of algae oil produces the preparation method of HC fuel.
Background technology
Along with industry and economic fast development, energy shortage and environmental problem are day by day serious, seek a kind of cleaning, renewable
, the new forms of energy of alternative fossil energy be the problem that the mankind need solution badly.Solar energy, wind energy, underground heat, biomass energy etc. are each
Planting in new forms of energy, biomass energy is unique a kind of new forms of energy that can produce liquid fuel.
The production ways of biomass energy mainly has three: animals and plants, microbial grease produce biodiesel by ester-exchange technology,
Starch, cellulose pass through producing fuel ethyl alcohol by ferment, and wood flour, straw etc. produce bio oil by heat/catalytic pyrolysis.Biodiesel
Main component be fatty acid methyl ester, biomass cracked oil also contains a large amount of esters, organic acid and aldehyde compound, therefore,
Their oxygen content is high.High oxygen content can cause the poor storage stability of oil product, viscosity height, calorific value is low, ignition performance is poor,
Thus limit its application.
At present, the method for oils and fats deoxidation mainly has hydrogenation and decarboxylation two kinds.Oil hydrogenation is mainly under catalyst action, oils and fats
Reacting with hydrogen, the oxygen in oils and fats removes with the form of water.Oils and fats decarboxylic reaction is mainly under the effect of catalyst, oil
Oxygen in fat is with CO2Form removing.The hydrogenation deoxidation of oils and fats needs the atmosphere of hydrogen, and course of reaction needs to consume hydrogen, and
And need the noble metal catalysts such as higher hydrogen pressure (3Mpa-10Mpa) and temperature (200 DEG C-600 DEG C), and Pd/Pt.Oil
The decarboxylation of fat does not consume hydrogen, only need to provide the environment of an anaerobic, and reaction pressure is relevant with the activity of used catalyst, and one
As at 0.5Mpa, far below the pressure of hydrogenation deoxidation.The present invention uses the oxygen in the method removing oils and fats of catalytic decarboxylation, it is provided that one
Plant high activity, non-noble metal decarboxylation catalyst, make oils and fats decarboxylation procedure carry out at ambient pressure, both reduced catalyst and equipment
Cost of investment, improves the safety of operation, has again high oils and fats DNA vaccine and liquid hydrocarbon productivity.It addition, the present invention not only may be used
With with common animal and plant fat and their methyl ester compound as raw material, it is also possible to algae oil and methyl ester compound thereof as raw material, change
The oxygen content of oils and fats and correlated performance so that it is meet the requirement of fuel applications.
Summary of the invention
The shortcoming that the invention solves the problems that above-mentioned prior art, it is provided that a kind of algae oil produces the preparation method of HC fuel, a kind of low liquid
The preparation method of state HC fuel, will solve the problem in that preparation a kind of high activity, non-precious metal catalyst, and this catalyst is permissible
Make oils and fats in normal pressure nitrogen atmosphere, occur at a lower temperature decarboxylic reaction, the method have higher oils and fats DNA vaccine and
Liquid hydrocarbon productivity, and can be with various animals and plants, microbial greases such as algae oil as raw material, the strong adaptability of raw material.
The present invention solves the technical scheme that its technical problem uses: this algae oil produces the preparation method of HC fuel, the method bag
Include following steps: in nitrogen atmosphere, by oil compounds by being pumped into the pipe reaction equipped with supported molybdenum catalyst
Device carries out catalytic decarboxylation reaction, obtains HC fuel；The reaction atmosphere of described decarboxylation deoxidation reaction is nitrogen, reaction pressure
For normal pressure, reaction temperature is 300-360 DEG C, and the response time is 1.5-3.0h, and feed rate is 0.03-0.30g/(cm2Min)；
Wherein said supported molybdenum catalyst is with molybdenum as active metal, with activated carbon as catalyst carrier.
Described oil compounds is algae oil and the mixed methyl aliphatic ester prepared of algae oil.
Described supported molybdenum catalyst is prepared as follows: the absorbent charcoal carrier handled well is impregnated into molybdenum catalyst forerunner
In the aqueous solution of body, calcining after drying, after calcining, logical Hydrogen activation, obtains molybdenum C catalyst；Wherein molybdenum catalyst precursor is
Ammonium Molybdate Tetrahydrate, calcining heat is 400 DEG C, and calcination time is 2 hours；Activation temperature is 400 DEG C, and soak time is 3 little
Time, Mo load factor on the activated carbon is 15-50%.
The invention have the advantages that: compared with prior art, the support type with activated carbon as carrier used due to the present invention
The catalysis activity of molybdenum catalyst is high, and reaction condition is gentle, and the ester conversion rate obtained, DNA vaccine and liquid hydrocarbon productivity are higher.Experiment
Result shows, the preparation method that the present invention provides is at normal pressure, nitrogen atmosphere, and Mo load factor on the activated carbon is 15%-50%,
Reaction temperature is 300-360 DEG C, and feed rate is 0.03-0.30g/(min cm2), under conditions of time of staying 1.5h 3.0h,
The conversion ratio of raw oil is 34.8%-99.3%, and DNA vaccine is 34.3%-99.1%, and liquid hydrocarbon productivity is about 46.1%-78.6%.
Accompanying drawing explanation
Fig. 1 is reaction unit figure；
Fig. 2 is the GC-MS figure of algae oil methyl ester (reaction raw materials)；
Fig. 3 is the GC-MS figure of liquid product prepared by the embodiment of the present invention；
Detailed description of the invention
Being clearly and completely described the technical scheme in embodiment of the present invention below, described embodiment is only this
Invent a part of example rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
There is on the premise of making creative work the every other embodiment obtained, broadly fall into the scope of protection of the invention.
The invention discloses a kind of algae oil and produce the preparation method of HC fuel, the method comprises the following steps: in nitrogen atmosphere,
By oil compounds by being pumped into, equipped with the tubular reactor of supported molybdenum catalyst carries out catalytic decarboxylation reaction, obtaining
HC fuel；The reaction atmosphere of described decarboxylation deoxidation reaction is nitrogen, and reaction pressure is normal pressure, and reaction temperature is 300-360 DEG C,
Response time is 1.5-3.0h, and feed rate is 0.03-0.30g/(cm2Min)；Wherein said supported molybdenum catalyst with molybdenum is
Active metal, with activated carbon as catalyst carrier.
In the present invention, described oils and fats is from the oils and fats of extraction in microalgae.
This supported molybdenum catalyst is with metal molybdenum as active component, and meanwhile, catalyst carrier selects the activated carbon that specific surface area is big,
Synergism between metal molybdenum and absorbent charcoal carrier, substantially increases the activity of catalysis.Concrete principle is, the ester group in oils and fats and mistake
Crossing generation complexation reaction of formation intermediate between metal molybdenum, at a certain temperature, ester bond departs from parent molecule, and with dioxy
The form changing carbon is discharged；While ester bond departs from parent molecule, parent molecule generates hydrocarbon, and molybdate compound is reduced to metal
Molybdenum.
Compared with prior art, owing to the present invention uses the supported molybdenum catalyst using activated carbon as catalyst carrier, catalysis
Agent activity is higher, under the molybdenum synergism with carrier, reduces the reaction condition of oils and fats decarboxylation deoxidation reaction, and reaction is with nitrogen
For carrier gas, carry out at ambient pressure, greatly reduce production cost, add the safety of production.
In order to further illustrate technical scheme, below in conjunction with embodiment, the preferred embodiment of the invention is described,
It is understood that these describe simply as further illustrating the features and advantages of the present invention rather than to the claims in the present invention
Restriction.
1) preparation of catalyst
The supported molybdenum catalyst that the present invention uses preferably is prepared according to infusion process, is more preferably prepared as follows: will be dried
Absorbent charcoal carrier be impregnated in the aqueous solution of molybdenum catalyst precursor, calcine after drying, after calcining, logical hydrogen reducing, is born
Load type molybdenum catalyst.Described molybdenum catalyst precursor is preferably Ammonium Molybdate Tetrahydrate；Described baking temperature is 70 DEG C, drying time
For 5h；Described calcining heat is 400 DEG C, and calcination time is 2h；Described reduction pressure is normal pressure, and hydrogen flowing quantity is 100ml/min,
Reduction temperature is 400 DEG C, and the recovery time is 3h.The preparation method of above-mentioned supported molybdenum catalyst is easy and simple to handle, to equipment requirements
Simply, catalyst preparation is repeatable high, it is easy to industrialized production.
Embodiment 1
30g Ammonium Molybdate Tetrahydrate is joined in 100mL distilled water, stirring and dissolving, obtain ammonium molybdate aqueous solution.
Being joined by absorbent charcoal carrier dried for 20g in described ammonium molybdate solution, at 25 DEG C, stirring dipping 2h, stands overnight,
Sucking filtration removes the supernatant, and gained filter cake is dried to constant weight at 70 DEG C, and it is anti-that its method as shown in Figure 1 is packed into tubular type
Answer in device.Logical nitrogen calcines 2h at 400 DEG C, then leads to hydrogen and reduce 3h at 400 DEG C, obtains the Mo-C that load factor is 40%
Catalyst.
Embodiment 2
20g Ammonium Molybdate Tetrahydrate is joined in 100mL distilled water, stirring and dissolving, obtain ammonium molybdate aqueous solution.
Being joined by absorbent charcoal carrier dried for 20g in described ammonium molybdate solution, other operation, with embodiment 1, is loaded
Rate is the Mo-C catalyst of 27%.
Embodiment 3
15g Ammonium Molybdate Tetrahydrate is joined in 100mL distilled water, stirring and dissolving, obtain ammonium molybdate aqueous solution.
Being joined by absorbent charcoal carrier dried for 20g in described ammonium molybdate solution, other operation, with embodiment 1, is loaded
Rate is the Mo-C catalyst of 18%.
Embodiment 4
30g Ammonium Molybdate Tetrahydrate is joined in 100mL distilled water, stirring and dissolving, obtain ammonium molybdate aqueous solution.
Being joined by silica supports dried for 20g in described ammonium molybdate solution, other operation, with embodiment 1, is born
Load rate is the Mo-SiO of 34.8%2Catalyst.
Embodiment 5
20g Ammonium Molybdate Tetrahydrate is joined in 100mL distilled water, stirring and dissolving, obtain ammonium molybdate aqueous solution.
By Al dried for 20g2O3Carrier joins in described ammonium molybdate solution, and other operation, with embodiment 1, obtains load factor
It is the Mo-Al of 23.7%2O3Catalyst.
Embodiment 6
By 50g Mg(NO3)26H2O joins in 100mL distilled water, and stirring and dissolving obtains magnesium nitrate aqueous solution.
By Al dried for 20g2O3Carrier joins in described magnesium nitrate solution, and at 25 DEG C, stirring dipping 2h, stands overnight,
Sucking filtration removes the supernatant, and gained filter cake is dried to constant weight at 70 DEG C；Put into Muffle furnace, at 450 DEG C, calcine 12h.?
It is the MgO-Al of 20.0% to load factor2O3Catalyst.
2) decarboxylic reaction prepares liquid hydrocarbon fuels
Embodiment 1
Method as shown in Figure 1, first to 60cm length, external diameter 20mm, the tubular reactor of internal diameter 16mm loads 10g quartz
Sand, then loads the Mo-C catalyst that 20g load factor is 40% on quartz sand, and height is about 12cm, finally at catalyst
Top remaining space loads quartz sand；Open heating and temperature control equipment, the quartz sand in tubular reactor and catalyst are added
Heat also maintains 340 DEG C (reaction temperatures)；By fuel oil preheating to 70 DEG C, by pump with 0.08g/(cm2Min) charging
Speed is transported to tubular reactor from top；Through condensing tube, (condensation temperature is the material flowed out from tubular reactor lower end
25 DEG C) cooling obtain liquid product；The liquid product collected, weighs, with the most unreacted fatty acid of gas chromatographic analysis
The content of methyl ester, and the composition of liquid hydrocarbon that generates and content, calculate the conversion ratio of raw material, according to formula (2) according to formula (1)
Calculate DNA vaccine, calculate liquid hydrocarbon productivity according to formula (3).
Under operating condition described in embodiment 1, conversion ratio is 91.2%, and DNA vaccine is 91.1%, and liquid hydrocarbon productivity is about 79.6%.
Embodiment 1 is prepared product liquid and carries out GC-MS analysis, result as it is shown on figure 3, it can be seen that
This product is mainly the hydrocarbon compound of C15, C17, and raw fatty acid methyl ester substantially completely converts.
Other embodiments
Operating parameter and the result of other embodiments are different from embodiment 1, but operational approach and process are with embodiment 1.Table 1 arranges
Go out the result under different operating parameter.
The operating parameter of each embodiment of table 1 and result
Comparative example
Catalyst used in comparative example is different from embodiment, respectively with 34.8% Mo-SiO2, the Mo-Al of 23.7%2O3With
The MgO-Al of 20.0%2O3For catalyst, operating process and the operational approach of reaction are same as in Example 1.Table 2 compares respectively
The liquid hydrocarbon condition of production in the case of catalyst.
Table 2 different catalysts effectiveness comparison
In addition to the implementation, the present invention can also have other embodiments.The skill that all employing equivalents or equivalent transformation are formed
Art scheme, all falls within the protection domain of application claims.
Claims (1)
1. the preparation method of an algae oil production HC fuel, it is characterized in that: the method comprises the following steps: in nitrogen atmosphere, by oil compounds by being pumped into, equipped with the tubular reactor of supported molybdenum catalyst carries out catalytic decarboxylation reaction, obtaining HC fuel；The reaction atmosphere of described decarboxylation deoxidation reaction is nitrogen, and reaction pressure is normal pressure, and reaction temperature is 300-360 DEG C, and the response time is 1.5-3.0h, and feed rate is 0.03-0.30g/(cm2Min)；Wherein said supported molybdenum catalyst is with molybdenum as active metal, with activated carbon as catalyst carrier；Described oil compounds is algae oil and the mixed methyl aliphatic ester prepared of algae oil；Described supported molybdenum catalyst is prepared as follows: is impregnated in the aqueous solution of molybdenum catalyst presoma by the absorbent charcoal carrier handled well, calcines after drying, and after calcining, logical Hydrogen activation, obtains molybdenum C catalyst；Wherein molybdenum catalyst precursor is Ammonium Molybdate Tetrahydrate, and calcining heat is 400 DEG C, and calcination time is 2 hours；Activation temperature is 400 DEG C, and soak time is 3 hours, and Mo load factor on the activated carbon is 15-50%.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104403683A (en) * | 2014-11-14 | 2015-03-11 | 浙江大学 | Method for using non-noble metal catalyst to catalyze decarboxylation of saturated fatty acid to prepare long-chain alkane |
| CN105567285B (en) * | 2016-03-04 | 2017-08-01 | 浙江大学 | A kind of method for preparing long chain alkane and aromatic hydrocarbons simultaneously by raw material of gutter oil |
| CN105670679B (en) * | 2016-03-04 | 2017-08-01 | 浙江大学 | A kind of method for preparing long chain alkane and aromatic hydrocarbons simultaneously by raw material of oleic acid |
| CN105567284B (en) * | 2016-03-04 | 2017-08-01 | 浙江大学 | A kind of method that long chain alkane and aromatic hydrocarbons are prepared with microalgae oil simultaneously for raw material |
| CN108586181B (en) * | 2018-05-21 | 2021-09-21 | 华东师范大学 | Method for decarbonylating grease into long-chain alkane under hydrogen-free condition |
| CN109052320A (en) * | 2018-08-24 | 2018-12-21 | 上海理工大学 | A kind of method that microalgae alkali extraction heat oil prepares hydrogen |
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