CN109482212A - A kind of preparation and its biomass hydrogenation deoxidation application of low temperature self assembly molybdenum carbide nano-wire catalyst - Google Patents
A kind of preparation and its biomass hydrogenation deoxidation application of low temperature self assembly molybdenum carbide nano-wire catalyst Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention provides a kind of preparation of low temperature self assembly molybdenum carbide nano-wire catalyst and its biomass hydrogenation deoxidation applications, belong to biomass energy science and technology field.I.e. using oxygen-containing molybdenum source aqueous solution and nitrogen-containing heterocycle compound as raw material, through self assembly, low temperature pyrogenation controllable preparation molybdenum carbide nano-wire catalyst.The method achieve the ultralow temperature of the molybdenum carbide nano wire of different stoichiometric ratios without template controllable preparation, and material storage is abundant, and easy to operate, technical process is simply controllable, is suitable for large-scale production.Prepared molybdenum carbide nano-wire catalyst in biomass, as benzofuran, diphenyl ether, fatty acid hydrogenation deoxidation in have good application prospect.
Description
Technical field
The invention belongs to biomass energy science and technology fields, are related to a kind of low temperature self assembly molybdenum carbide nanowire catalytic
Agent and its biomass hydrogenation deoxidation application.In particular, using oxygen-containing molybdenum source aqueous solution and nitrogen-containing heterocycle compound as raw material, through certainly
Assembling, low temperature pyrogenation (< 500 DEG C) controllable preparation molybdenum carbide nano-wire catalyst, can realize biomass, such as benzene in a mild condition
And the highly effective hydrogenation deoxidation of furans, diphenyl ether, fatty acid.This method can realize the molybdenum carbide nano wire of different stoichiometric ratios
Ultralow temperature is without template controllable preparation, and material storage is abundant, and easy to operate, technical process is simply controllable, is suitable for extensive raw
It produces, has a good application prospect in biomass conversion field.
Background technique
Petroleum reserves constantly declines at present, and energy crisis has become one that people must face and extremely serious asks
Topic, we continually develop new energy to meet the growing energy demand of people thus.Biomass can be again as a kind of cleaning
The raw energy, quilt is it is believed that be a kind of very potential substitute energy source for petroleum.But in biomass containing a large amount of acid, phenol,
The oxygenatedchemicals such as furans account for about the half or so of all substances content, low so as to cause its fuel value, stability is bad simultaneously
With corrosivity.This allows for its application and is restricted, in order to can sufficiently be applied, while alleviating energy crisis,
Our top priorities are exactly to carry out hydrogenation deoxidation to it to reduce its oxygen content.Biomass refers to all utilization Plant Light cooperations
With the organic substance of formation, range is extremely wide can to grow lived organism including all.Wherein have much representativeness
Be exactly plant and animal wastes.It stores solar energy in organism in the form of chemical energy, referred to as biomass energy,
This energy has the features such as low pollution, renewable and widely distributed.Therefore deoxidation purification must be carried out to biomass energy, mentioned
High energy source utilization rate.In general, the catalyst of industrial hydrogenation deoxidation (HDO) is all derived from hydrodesulfurization (HDS) catalysis
Agent.Therefore the type of hydrogenation deoxidation catalysts is relatively abundanter, has load type double-metal sulfide or bimetallic alloy to urge
Agent such as Ni-Mo/Al2O3、NiMoSxDeng there are also noble metal catalyst Pt, Ru etc..Noble metal catalyst higher cost, metal sulphur
Compound activity is lower.Therefore need to find a kind of catalyst to solve these problems.It is anti-that transition metal carbide in many relates to hydrogen
Should such as ammonia synthesis and decomposition, hydrodesulfurization (HDS), the catalytic property that class noble metal is all shown in hydrodenitrogeneration (HDN),
And its cost is relatively low, so that it be made to have very wide application prospect in terms of hydrogenation deoxidation.
Transition metal carbide is to fill compound between the metal of formation in carbon atom insertion metal lattice.Due to carbon atom
Insertion, cause spacing of lattice to increase, lattice parameter becomes larger, so as to cause metal d band shrink, fermi level d electron density increase
Add, so that it be made to show the property of class noble metal.Therefore, for carbide especially molybdenum carbide because its is cheap, reserves are rich
The features such as rich, causes the concern of more and more people.In numerous hydrogen-involved reactions, molybdenum carbide has shown urging for its class noble metal
Change performance, is also considered as very potential noble metal catalyst substitute.
The method for synthesizing molybdenum carbide is varied, and new molybdenum carbide preparation method emerges one after another.Generally speaking, molybdenum carbide
Synthetic method mainly has 3 kinds of methods: (1) carbothermic method, by molybdenum salt and solid carbon such as carbon black, after the mixing such as active carbon again
High-temperature calcination (US2285837, US4914070), high temperature are easy to be sintered molybdenum carbide particles and cause serious carbon layer on surface
Covering and low specific surface area.(2) temperature-programmed reduction method, be the light hydrocarbons such as the oxide and methane of molybdenum, ethane or
The process that temperature programming program is carbonized is set under light hydrocarbons and hydrogen mixed gas atmosphere, and this method is easy to operate but is carbonized
Carbon distribution can be still generated under gas high temperature, covering active sites reduce specific surface area.(3) microwave thermal solution, this method are to carbon heat
The improvement of reduction method is mixed with metal molybdenum or molybdenum oxide with solid carbon, prepared in 90 seconds using microwave heating
Obtain single-phase molybdenum carbide.This method preparation time is short, and material granule is small and uniform, but still has that carbon is remaining to ask
Topic.In addition there are chemical vapor deposition, hydro-thermal method, single-source precursor methods etc..However, above-mentioned synthesizing mean is quickly and easily being prepared
Still there is some problems in terms of the molybdenum carbide catalyst haveing excellent performance with morphology controllable.
Summary of the invention
The present invention is intended to provide a kind of low temperature self assembly molybdenum carbide nano-wire catalyst and its biomass hydrogenation deoxidation application.
The preparation method simple process of the molybdenum carbide nano-wire catalyst, low in cost, low energy consumption, in biomass, such as benzofuran, two
There is high catalytic activity and stability in the reaction of the hydrogenation deoxidations such as phenylate, fatty acid, to a certain extent effectively instead of your gold
Metal catalyst.
Technical solution of the present invention:
A kind of preparation method of low temperature self assembly molybdenum carbide nano-wire catalyst, steps are as follows:
Molybdic acid saline solution is uniformly mixed with nitrogen-containing heterocycle compound, reconciles 10-110 DEG C of temperature, adjusting pH is 6.5-
3, the self assembly of reaction time 4-60h obtains organic precursor containing molybdenum;By the substance of collection one of argon gas or argon gas with
In the gaseous mixture of hydrogen, at 450-700 DEG C, constant temperature 1-4h hours, step pyrolysis obtained molybdenum carbide nano-wire catalyst.
The molar ratio of the nitrogen-containing heterocycle compound and Mo is 0.5-3, wherein optimal ratio is 0.8-1.5.
The molybdate is ammonium molybdate, phosphomolybdic acid, sodium molybdate or silicomolybdic acid.
The nitrogen-containing heterocycle compound is 3- amino-1,2,4-triazol or triazole derivatives.
Prepared molybdenum carbide nano-wire catalyst in biomass, as benzofuran, diphenyl ether, fatty acid hydrogenation deoxidation
There is high catalytic activity and stability, DNA vaccine is up to 100% in reaction.
Beneficial effects of the present invention: low temperature self assembly of the present invention prepares the molybdenum carbide of different-shape and Mo/C ratio
Method, preparation process simply easily realize that easy to operate, safety, technological parameter is easily controllable, obtain molybdenum carbide catalyst with line
Shape, rectangle, band-like equal different morphologies are not necessarily to additional template agent, and pyrolysis temperature is extremely low, can be applied to biomass conversion such as benzo
Furans, diphenyl ether in aliphatic acid hydrogenation deoxygenation, and show good catalytic effect.
Detailed description of the invention
Fig. 1 is the XRD diagram of the precursor molybdenum carbide that 460 degree of pyrolysis 4h are obtained under argon gas and hydrogen mixed gas in the present invention
Fig. 2 is the SEM figure for the molybdenum carbide nano wire that 460 degree of pyrolysis 4h are obtained under mixed atmosphere in the present invention
Specific embodiment
The present invention will be described in detail below by embodiment, but the invention is not limited to these embodiments.
Embodiment 1
1.2358g ammonium molybdate is dissolved in 60mL deionized water, and 0.4708g 3- amino -1,2,4- triazole is added to above-mentioned molten
In liquid, faint yellow clear solution is obtained after completely dissolution;Above-mentioned mixed liquor is persistently stirred into 12h, no Precipitation at 70 DEG C.
Embodiment 2
1.2358g ammonium molybdate is dissolved in 60mL deionized water, and 0.4708g 3- amino -1,2,4- triazole is added to above-mentioned molten
In liquid, faint yellow clear solution is obtained after completely dissolution;Above-mentioned mixed liquor is persistently stirred into 12h at 70 DEG C, is obtained light yellow
Precipitating is collected by filtration and in 80 DEG C of at a temperature of drying in precipitating;Quartz boat equipped with buff powder is put into tube furnace,
In the mixed atmosphere that argon gas is 40mL/ points and hydrogen is 20mL/ points, 460 DEG C are warming up to 5 DEG C/minute of heating rate, constant temperature 4
Hour, gas is closed, carbonization molybdenum material is obtained after natural cooling.The molybdenum carbide of preparation is subjected to SEM characterization, obtains Fig. 2 nanometer
Line.
Embodiment 3
1.2358g ammonium molybdate is dissolved in 60mL deionized water, and 0.7063g 3- amino -1,2,4- triazole is added to above-mentioned molten
In liquid, faint yellow clear solution is obtained after completely dissolution;Above-mentioned mixed liquor is persistently stirred into 12h at 70 DEG C, is obtained light yellow
Precipitating is collected by filtration and in 80 DEG C of at a temperature of drying in precipitating;Quartz boat equipped with buff powder is put into tube furnace,
In the mixed atmosphere that argon gas is 40mL/ points and hydrogen is 20mL/ points, 460 DEG C are warming up to 5 DEG C/minute of heating rate, constant temperature 4
Hour, gas is closed, carbonization molybdenum material is obtained after natural cooling.The molybdenum carbide of preparation is subjected to XRD characterization, obtains Fig. 1.
Embodiment 3
1.2358g ammonium molybdate is dissolved in 60mL deionized water, and 0.7063g 3- amino -1,2,4- triazole is added to above-mentioned molten
In liquid, faint yellow clear solution is obtained after completely dissolution;Above-mentioned mixed liquor is persistently stirred into 12h at 10 DEG C, is obtained light yellow
Precipitating is collected by filtration and in 80 DEG C of at a temperature of drying in precipitating;Quartz boat equipped with buff powder is put into tube furnace,
Argon gas is that 40mL/ divides in inert atmosphere, is warming up to 500 DEG C with 5 DEG C/minute of heating rate, constant temperature 2 hours, closes gas, natural
Carbonization molybdenum material is obtained after cooling.
Embodiment 4
1.2358g ammonium molybdate is dissolved in 60mL deionized water, and 0.7063g 3- amino -1,2,4- triazole is added to above-mentioned molten
In liquid, faint yellow clear solution is obtained after completely dissolution;Above-mentioned mixed liquor is persistently stirred into 12h at 110 DEG C, is obtained light yellow
Precipitating is collected by filtration and in 80 DEG C of at a temperature of drying in precipitating;Quartz boat equipped with buff powder is put into tube furnace,
Argon gas is that 40mL/ divides in inert atmosphere, is warming up to 500 DEG C with 5 DEG C/minute of heating rate, constant temperature 2 hours, closes gas, natural
Carbonization molybdenum material is obtained after cooling.
Embodiment 5
1.2358g ammonium molybdate is dissolved in 60mL deionized water, 0.7063g 3- amino -1,2 at 10 DEG C, and 4- triazole is added
Into above-mentioned solution, faint yellow clear solution is obtained after completely dissolution;Solution PH is reconciled by acetic acid to be 6.5 and hold at 10 DEG C
Continuous stirring 12h, obtains light-yellow precipitate, is collected by filtration and in 80 DEG C of at a temperature of drying;The quartz of buff powder will be housed
Boat is put into tube furnace, is that 40mL/ divides in inert atmosphere in argon gas, is warming up to 500 DEG C with 5 DEG C/minute of heating rate, constant temperature 2
Hour, gas is closed, carbonization molybdenum material is obtained after natural cooling.
Embodiment 6
1.2358g ammonium molybdate is dissolved in 60mL deionized water, 0.7063g 3- amino -1,2 at 10 DEG C, and 4- triazole is added
Into above-mentioned solution, faint yellow clear solution is obtained after completely dissolution;Solution PH is reconciled by acetic acid to be 3 and continue at 10 DEG C
12h is stirred, light-yellow precipitate is obtained, is collected by filtration and in 80 DEG C of at a temperature of drying;The quartz boat of buff powder will be housed
It is put into tube furnace, is that 40mL/ divides in inert atmosphere in argon gas, is warming up to 500 DEG C with 5 DEG C/minute of heating rate, constant temperature 2 is small
When, gas is closed, carbonization molybdenum material is obtained after natural cooling.
Implement 7
Molybdenum carbide catalyst in embodiment 3 is applied in aliphatic acid hydrogenation deoxygenation, 0.05g molybdenum carbide nanometer is taken
Line, the 4MPa hydrogen in fixed bed reactors carry out hydrogenation deoxidation, conversion ratio and deoxidation to 1.2% palmitic acid at 330 DEG C
For conversion ratio all close to 100%, paraffin selectivity is up to 99.2%
Implement 8
Molybdenum carbide catalyst in embodiment 3 is applied in the reaction of diphenyl ether hydrogenation deoxidation, 0.1g molybdenum carbide nanometer is taken
Line, the 0.5MPa hydrogen in fixed bed reactors carry out hydrogenation deoxidation, conversion ratio and deoxidation to 5% diphenyl ether at 280 DEG C
For conversion ratio all close to 100%, the selectivity of benzene is up to 95.4%
Implement 9
Molybdenum carbide catalyst in embodiment 3 is applied in the reaction of diphenyl ether hydrogenation deoxidation, 0.1g molybdenum carbide nanometer is taken
Line, the 3MPa hydrogen in fixed bed reactors carry out hydrogenation deoxidation to 5% benzofuran at 320 DEG C, and conversion ratio is
97.8% and deoxidation conversion ratio all close to 100%, the selectivity of ethylo benzene is up to 92.4%.
Claims (7)
1. a kind of preparation method of low temperature self assembly molybdenum carbide nano-wire catalyst, which is characterized in that steps are as follows:
Molybdic acid saline solution is uniformly mixed with nitrogen-containing heterocycle compound, reconciles 10-110 DEG C of temperature, adjusting pH is 6.5-3, instead
4-60h self assembly obtains organic precursor containing molybdenum between seasonable;By the substance of collection in one of argon gas or argon gas and hydrogen
Gaseous mixture in, at 450-700 DEG C, constant temperature 1-4h hours, a step pyrolysis obtain molybdenum carbide nano-wire catalyst.
2. preparation method according to claim 1, which is characterized in that the molar ratio of the nitrogen-containing heterocycle compound and Mo
For 0.5-3.
3. preparation method according to claim 1, which is characterized in that the molar ratio of the nitrogen-containing heterocycle compound and Mo
For 0.8-1.5.
4. preparation method according to claim 1 to 3, which is characterized in that the molybdate is ammonium molybdate, phosphorus molybdenum
Acid, sodium molybdate or silicomolybdic acid.
5. preparation method according to claim 1 to 3, which is characterized in that the nitrogen-containing heterocycle compound is 3- ammonia
Base -1,2,4- triazole or triazole derivatives.
6. the preparation method according to claim 4, which is characterized in that the nitrogen-containing heterocycle compound is amino -1 3-,
2,4- triazole or triazole derivatives.
7. hydrogenation deoxidation of the above-mentioned molybdenum carbide nano-wire catalyst for biomass reacts.
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CN113200807A (en) * | 2021-05-12 | 2021-08-03 | 中国科学院山西煤炭化学研究所 | Method for preparing high-purity C16 and C18 normal mono-alkane |
CN114214640A (en) * | 2022-01-18 | 2022-03-22 | 武汉科技大学 | Biomass carbon-based nano molybdenum carbide-molybdenum nitride heterojunction composite catalyst and method |
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CN114214640A (en) * | 2022-01-18 | 2022-03-22 | 武汉科技大学 | Biomass carbon-based nano molybdenum carbide-molybdenum nitride heterojunction composite catalyst and method |
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