CN103936008A - Synthesis method of nano-molybdenum carbide - Google Patents
Synthesis method of nano-molybdenum carbide Download PDFInfo
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Abstract
The invention relates to a synthesis method of nano-molybdenum carbide. The synthesis method comprises the following steps: dissolving a molybdenum precursor in hydrogen peroxide, dissolving carbohydrates in water, mixing the molybdenum precursor with the carbohydrates, stirring, loading a mixed solution into a hydrothermal kettle, and performing hydrothermal treatment to obtain a black product; cooling the black product, then washing and performing suction filtration on the product, drying, baking in a passivation gas atmosphere, replacing with passivation gas when the temperature is reduced to room temperature, and performing passivation treatment to obtain the nano-molybdenum carbide. The synthesis method provided by the invention has the advantages of simplicity, easiness in control, economical efficiency, reasonableness and large specific surface area with mesoporous structure.
Description
Technical field
The invention belongs to nano material preparation, be specifically related to a kind of rice molybdenum carbide synthetic method.
Background technology
Transition metal carbide be carbon atom enter the lattice of transition metal and the class that produces have metalline between fill compound, it has shown the denominator of covalency solid, ionic crystal and transition metal, thereby there is special physics and chemistry character, be embodied in high-melting-point and hardness, high stability and mechanical stability and have good erosion resistance, it also has and similarly electricity, magnetic property and be widely used in the essential industry such as mining industry, machinery industry field of its parent metal in addition.Since nineteen seventies it is found that transition metal carbide has the character of class precious metal in a series of catalyzed reactions, transition metal carbide causes people's very big concern in catalytic science as a class new catalytic material.Particularly grow to even greater heights at the cry efficient and greenization utilization that is accompanied by oil price rise fast, the energy and resource in recent years, the exploitation of carbides catalytic performance and new catalyzed reaction has further been promoted to the concern of people to carbide.In addition, because carbide synthesis material is comparatively cheaply easy to get, saving precious metal precious resources, reduce catalyzed reaction cost also significant.And molybdenum carbide especially attracts much attention.
Molybdenum carbide is described as " accurate platinum catalyst ", and it has the electronic structure of class precious metal, thereby has similar catalytic performance with platinum family precious metal to a great extent, shows especially suitable with the precious metal such as Pt, Pd in hydrogenation catalyst performance.Along with the research of molybdenum carbide is goed deep into, find molybdenum carbide at the lower carbon number hydrocarbons such as water-gas shift, methane and CO 2 reformation, methanol vapor reformation, methanol electro-oxidizing, for direct methanol fuel cell, fischer-tropsch is synthetic, alcohol mixture is synthetic, the reaction such as isomerization, aromizing of the hydrogenating desulfurization of oil product and hydrodenitrification, olefin metathesis, hydrogenation/dehydrogenation, hydro carbons all has fine performance, in the energy and chemical industry catalyzed reaction, has shown great potential.Compared with noble metal catalyst, it is high that molybdenum carbide has cheap and anti-sulphur, is expected to become a kind of novel hydrogenation and selective hydrogenation catalyst, especially CO hydrogenation aspect.
Along with going deep into of research, the new method of preparing molybdenum carbide is also constantly proposing and is being verified.At present the preparation method of molybdenum carbide mainly contains following several: (1) temperature programming reaction method, by molybdenum oxide precursor at light hydrocarbon or light hydrocarbon/H
2gas mixture Program intensification carbonization (TPRe), the method easily control and product purer, but the method easily causes catalyst surface carbon distribution, and gained molybdenum carbide specific surface area is little.(2) carbothermic method, is reacted in protective atmosphere or reducing atmosphere by molybdenum oxide and appropriate carbon support, and the product that the method obtains has compared with bigger serface, but this temperature of reaction is conventionally very high.(3) solvothermal method, the method is to adopt the strong material of reducing power (as KBH
4) molybdenum oxide is reduced to molybdenum carbide, the method is simple and easy to control, and temperature is low, but product is impure.(4) metallic precursor cracking process, is utilize organometallics and utilize the mixture Pintsch process of ammonium molybdate and hexamethylenetetramine to make, and product is purer, but precursor preparation is complicated, and it is larger to make particle.In addition also have the reports such as CVD, hydrothermal method, ultrasonic method, microwave method, but these methods exist equally output little, react the difficult problem such as insufficient, product particle is large, product is impure.Above method is limited to shortcoming own and particularly has larger deficiency aspect the volume production of catalyzer in practical application,
Summary of the invention
Objects of the present invention are to provide a kind of synthetic method of nano silicon carbide molybdenum of the bigger serface with meso-hole structure of simple and easy to control, economical rationality.
Synthetic method of the present invention comprises the steps:
(1) molybdenum precursor is dissolved in 30wt% hydrogen peroxide, molybdenum atom volumetric molar concentration is 0.001~1.0mol/L;
(2) glucide is soluble in water, concentration of saccharide is 0.3~5.0mol/L;
(3) be 1.0~100.0:1 by the mol ratio of carbohydrate and molybdenum atom, step (1) solution and step (2) are mixed and stirred;
(4) step (3) mixing solutions is packed in water heating kettle, at 100~250 DEG C, hydrothermal treatment consists 1~72 hour, obtains black product;
(5) black product cooling after by product washing, suction filtration, at 40~200 DEG C of temperature, dry 1~72 hour to dry;
(6) roasting under passivating gas atmosphere, maturing temperature is 500~1000 DEG C, roasting time 0.5~72 hour;
(7) in the time that temperature drops to room temperature, be replaced into passivating gas, passivation flow velocity is 5-20mL/min/gcat, and passivation temperature is 0~100 DEG C, and passivation time is 1~24 hour, can obtain nano silicon carbide molybdenum.
In step as above (1), molybdenum precursor can be the oxide compound of molybdate and molybdenum, and molybdate is ammonium molybdate, Sodium orthomolybdate or potassium molybdate, and the oxide compound of molybdenum is molybdenum dioxide or molybdic oxide.
Reaction in step as above (1) is to be 0~100 DEG C in temperature, and reaction is 20 minutes to 24 hours.
In step as above (2), glucide is glucose, sucrose, maltose or starch.
While stirring in step as above (3), keeping temperature is 0~100 DEG C, and churning time is 10 minutes to 24 hours.
In step (4), hydrothermal treatment consists temperature is preferably 140~220 DEG C as mentioned above, and constant temperature time is preferably 1~24 hour
In step (6), carburizing atmosphere is argon gas, nitrogen, helium, hydrogen, carbon monoxide, synthetic gas, methane gas as mentioned above, or the gas mixture of methane and hydrogen.
The gas flow of the carburizing atmosphere described in step (6) is 30~200mL/min/g cat. as mentioned above.
In step (6), maturing temperature is preferably 600~800 DEG C as mentioned above, and constant temperature time is preferably 0.5~24 hour.
The large specific surface nano silicon carbide molybdenum with meso-hole structure of the present invention, its specific surface area is high (is greater than 100m
2/ g), particle size little (3-10nm), be conducive to catalyzer in actual catalyzed reaction because nano effect shows excellent catalytic performance, and can need and carry out surface modification for actual catalyzed reaction, there is potentiality to be exploited and application prospect.
The porous nano molybdenum carbide of prepared by the inventive method have meso-hole structure is made up of molybdenum carbide nanoparticle, between nanoparticle, also there is abundant nano-pore structure, the molybdenum carbide particles of the porous nano molybdenum carbide with meso-hole structure of being prepared by the inventive method is little, and between particle, there is abundant meso-hole structure, specific surface area is large, between product, be connected by carbon is coated, play support dissemination, be conducive to the exposure of reactant diffusion and active sites: simultaneously, the nanotopography of class clad structure also helps the secondary assembling of catalyzer, creation has the multilevel ordered catalytic material of unique space structure, therefore the macropore molybdenum carbide of this meso-hole structure is expected at benzene hydrogenation, Fischer-Tropsch is synthetic, hydrogenating desulfurization/denitrogenation, alcohols decomposing hydrogen-production, the fine chemistry industry catalyzed reactions such as low-carbon alcohol is synthetic, with fuel cell electrode catalytic material, sensor, and apply in the field such as electricity and magnetics material.And the inventive method productive rate is very high, and preparation condition is simple and easy to control, processing condition cost is low, and preparation efficiency is high, and quality product and yield rate are high, has good application and industrialization prospect.
Brief description of the drawings:
Fig. 1 is the typical XRD spectra of the molybdenum carbide prepared of the present invention.
Fig. 2 is the typical transmission electron microscope photo of the molybdenum carbide material prepared of the present invention.
Fig. 3 is the typical isothermal nitrogen adsorption figure of the molybdenum carbide prepared of the present invention.
Embodiment
Embodiment 1
(1) 0.1g molybdic oxide is dissolved in the hydrogen peroxide of 10mL massfraction 30wt%, is placed under the water bath condition of 60 DEG C and stirs 2 hours;
(2) 10g glucose is dissolved in 100mL water;
(3) two solution in (1) (2) are mixed under the water bath condition that is placed on 40 DEG C and stirred 12 hours;
(4) solution obtaining in (3) is packed in 150mL self-pressure still, hydrothermal treatment consists 6 hours, obtains black product at 180 DEG C;
(5), by after cooling the black product obtaining in (4), be placed in baking oven and at 80 DEG C, dry 24 hours to dry with deionized water wash three times, filtration;
(6) by the product obtaining in (5) 700 DEG C of roastings 12 hours under the argon gas atmosphere of 30mL/min/gcat, temperature drops to 30 DEG C of postposition and is changed to 2.0vol.%O
2/ Ar passivating gas, Passivation Treatment 12h, flow velocity is 5mL/min/gcat.Gained sample is designated as MoC-1.Its thing phase parameter is in table 1.
Embodiment 2
(1) 2g ammonium molybdate is dissolved in the hydrogen peroxide of 20mL massfraction 30wt%, is placed under the water bath condition of 50 DEG C and stirs 2 hours;
(2) 25g sucrose is dissolved in 100mL water;
(3) two solution in (1) (2) are mixed under the water bath condition that is placed on 40 DEG C and stirred 12 hours;
(4) solution obtaining in (3) is packed in 150mL self-pressure still, hydrothermal treatment consists 6 hours, obtains black product at 170 DEG C;
(5), by after cooling the black product obtaining in (4), be placed in baking oven and at 80 DEG C, dry 24 hours to dry with deionized water wash three times, filtration;
(6) by the product obtaining in (5) 700 DEG C of roastings 12 hours under the argon gas atmosphere of 30mL/min/gcat, temperature drops to 30 DEG C of postposition and is changed to 2.0vol.%O
2/ Ar passivating gas, Passivation Treatment 12h, flow velocity is 10mL/min/gcat.Gained sample is designated as MoC-2.Its thing phase parameter is in table 1.
Embodiment 3
(1) 2g Sodium orthomolybdate is dissolved in the hydrogen peroxide of 20mL massfraction 30wt%, is placed under the water bath condition of 70 DEG C and stirs 2 hours;
(2) 30g maltose is dissolved in 100mL water;
(3) two solution in (1) (2) are mixed under the water bath condition that is placed on 40 DEG C and stirred 12 hours;
(4) solution obtaining in (3) is packed in 150mL self-pressure still, hydrothermal treatment consists 6 hours, obtains black product at 190 DEG C;
(5), by after cooling the black product obtaining in (4), be placed in baking oven and at 80 DEG C, dry 24 hours to dry with deionized water wash three times, filtration;
(6) by the product obtaining in (5) 700 DEG C of roastings 12 hours under the argon gas atmosphere of 30mL/min/gcat, temperature drops to 30 DEG C of postposition and is changed to 2.0vol.%O
2/ Ar passivating gas, Passivation Treatment 12 hours, flow velocity is 15mL/min/gcat.Gained sample is designated as MoC-3.Its thing phase parameter is in table 1.
Embodiment 4
(1) 1.5g potassium molybdate is dissolved in the hydrogen peroxide of 20mL massfraction 30wt%, is placed under the water bath condition of 80 DEG C and stirs 2 hours;
(2) 40g starch is dissolved in 100mL water;
(3) two solution in (1) (2) are mixed under the water bath condition that is placed on 40 DEG C and stirred 12 hours;
(4) solution obtaining in (3) is packed in 150mL self-pressure still, hydrothermal treatment consists 12 hours, obtains black product at 200 DEG C;
(5), by after cooling the black product obtaining in (4), be placed in baking oven and at 80 DEG C, dry 24 hours to dry with deionized water wash three times, filtration;
(6) by the product obtaining in (5) 700 DEG C of roastings 12 hours under the argon gas atmosphere of 30mL/min/gcat, temperature drops to 30 DEG C of postposition and is changed to 2.0vol.%O
2/ Ar passivating gas, Passivation Treatment 12 hours, flow velocity is 15mL/min/gcat.Gained sample is designated as MoC-1.Its thing phase parameter is in table 1.
Embodiment 5
(1) 1g molybdenum dioxide is dissolved in the hydrogen peroxide of 25mL massfraction 30wt%, is placed under the water bath condition of 70 DEG C and stirs 2 hours;
(2) 50g sucrose is dissolved in 100mL water;
(3) two solution in (1) (2) are mixed under the water bath condition that is placed on 40 DEG C and stirred 12 hours;
(4) solution obtaining in (3) is packed in 150mL self-pressure still, hydrothermal treatment consists 6 hours, obtains black product at 170 DEG C;
(5), by after cooling the black product obtaining in (4), be placed in baking oven and at 80 DEG C, dry 24 hours to dry with deionized water wash three times, filtration;
(6) H at 30mL/min/gcat by the product obtaining in (5)
2the lower 600 DEG C of roastings of atmosphere 12 hours, temperature drops to 30 DEG C of postposition and is changed to 2.0vol.%O
2/ Ar passivating gas, Passivation Treatment 12h, flow velocity is 20mL/min/gcat.Gained sample is designated as MoC-5.Its thing phase parameter is in table 1.
Embodiment 6
(1) 1.5g molybdic oxide is dissolved in the hydrogen peroxide of 20mL massfraction 30wt%, is placed under the water bath condition of 65 DEG C and stirs 2 hours;
(2) 20g glucose is dissolved in 100mL water;
(3) two solution in (1) (2) are mixed under the water bath condition that is placed on 40 DEG C and stirred 12 hours;
(4) solution obtaining in (3) is packed in 150mL self-pressure still, hydrothermal treatment consists 4 hours, obtains black product at 180 DEG C;
(5), by after cooling the black product obtaining in (4), be placed in baking oven and at 80 DEG C, dry 24 hours to dry with deionized water wash three times, filtration;
(6) H at 30mL/min/gcat by the product obtaining in (5)
2the lower 700 DEG C of roastings of atmosphere 6 hours, temperature drops to 30 DEG C of postposition and is changed to 2.0vol.%O
2/ Ar passivating gas, Passivation Treatment 12h, flow velocity is 20mL/min/gcat.Gained sample is designated as MoC-6.Its thing phase parameter is in table 1.
Because the molybdenum carbide particles of such nano silicon carbide molybdenum is little, and between particle, have abundant meso-hole structure, specific surface is large, and area carbon is few, is conducive to the exposure of reactant diffusion and active sites; Simultaneously, the coated shape nanotopography of class nucleocapsid also helps the secondary assembling of catalyzer, creation has the multilevel ordered catalytic material of unique space structure, the fine chemistry industry catalyzed reactions such as this nanocatalyst is expected to synthesize at benzene hydrogenation, Fischer-Tropsch, hydrogenating desulfurization/denitrogenation, alcohols decomposing hydrogen-production, with fuel cell electrode catalytic material, sensor, and apply in the field such as electricity and magnetics material.Because this product has above potential using value, and preparation condition is simple and easy to control, and processing condition cost is low, and preparation efficiency is high, and quality product and yield rate are high, and therefore this product has good application and industrialization prospect.In addition, the method has universality, can, by further regulating molybdenum source composition and carbohydrate carbon content and type etc., control the carbonization that obtains and plug with molten metal catalytic material composition and character, further the catalysis behavior of catalyzer that modulation forms.To the method systematic study, not only can provide the novel energy catalyzed conversion carbides catalytic material with class precious metal performance, and synthetic method and Catalyst Design to material has wide significance.
The physical properties of molybdenum carbide prepared by table 1 the present invention
Claims (11)
1. a synthetic method for nano silicon carbide molybdenum, is characterized in that comprising the steps:
(1) molybdenum precursor is dissolved in 30wt% hydrogen peroxide, molybdenum atom volumetric molar concentration is 0.001~1.0 mol/L;
(2) glucide is soluble in water, concentration of saccharide is 0.3~5.0 mol/L;
(3) be 1.0~100.0:1 by the mol ratio of carbohydrate and molybdenum atom, step (1) solution and step (2) are mixed and stirred;
(4) step (3) mixing solutions is packed in water heating kettle, at 100~250 DEG C, hydrothermal treatment consists 1~72 hour, obtains black product;
(5) black product cooling after by product washing, suction filtration, at 40~200 DEG C of temperature, dry 1~72 hour to dry;
(6) roasting under passivating gas atmosphere, maturing temperature is 500~1000 DEG C, roasting time 0.5~72 hour;
(7) in the time that temperature drops to room temperature, be replaced into passivating gas, passivation flow velocity is 5-20 mL/min/gcat, and passivation temperature is 0~100 DEG C, and passivation time is 1~24 hour, can obtain nano silicon carbide molybdenum.
2. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, is characterized in that in described step (1), molybdenum precursor is the oxide compound of molybdate and molybdenum.
3. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 2, is characterized in that described molybdate is ammonium molybdate, Sodium orthomolybdate or potassium molybdate.
4. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 2, is characterized in that the oxide compound of described molybdenum is molybdenum dioxide or molybdic oxide.
5. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, is characterized in that the reaction in described step (1) is to be 0~100 DEG C in temperature, and the reaction times is 20 minutes to 24 hours.
6. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, is characterized in that in described step (2), glucide is glucose, sucrose, maltose or starch.
7. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, while it is characterized in that the middle stirring of described step (3), keeping temperature is 0~100 DEG C, churning time is 10 minutes to 24 hours.
8. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, is characterized in that in described step (4), hydrothermal treatment consists temperature is 140~220 DEG C, and constant temperature time is 1~24 hour.
9. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, is characterized in that in described step (6), carburizing atmosphere is argon gas, nitrogen, helium, hydrogen, carbon monoxide, synthetic gas, methane gas, or the gas mixture of methane and hydrogen.
10. the synthetic method of a kind of nano silicon carbide molybdenum as claimed in claim 1, the gas flow that it is characterized in that the carburizing atmosphere described in described step (6) is 30~200 mL/min/g cat.
The synthetic method of 11. a kind of nano silicon carbide molybdenums as claimed in claim 1, is characterized in that in described step (6), maturing temperature is 600~800 DEG C, and constant temperature time is 0.5~24 hour.
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