CN107758668A - A kind of quick method for preparing carbon load molybdenum carbide of microwave heating - Google Patents
A kind of quick method for preparing carbon load molybdenum carbide of microwave heating Download PDFInfo
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Abstract
The present invention relates to carbon-based catalysis material preparing technical field, a kind of quick method for preparing carbon load molybdenum carbide of microwave heating, comprise the following steps：(1) preparation of presoma, (2) microwave radiation processing.Using the carbon load molybdenum carbide particle diameter distribution of the inventive method preparation is uniform, size is easily controllable, crystallinity is high, not oxidizable, stability is good.Have the advantages that applicability is extensive, green, technique is simple and safety, it is time-consuming it is short, energy consumption is low, is easy to large-scale production.
Description
Technical field
The present invention relates to a kind of quick method for preparing carbon load molybdenum carbide of microwave heating, belong to carbon-based catalysis material and prepare
Technical field.
Background technology
Transition metal carbide is that carbon atom enters the lattice of transition metal and caused a kind of had between metalline
Compound is filled, there are the special chemical and physical features such as fusing point is high and hardness is big, make it in fields such as the energy, catalysis and environment
It is widely applied.Wherein molybdenum carbide is because its is cheap, has electronic structure and the spy such as catalytic activity of class noble metal
Sign, is applied in numerous catalytic reactions frequently as the substitute of noble metal catalyst (Pt, Pd etc.), such as alkane isomerization, water
Gas conversion, hydrogenation of unsaturated hydrocarbons, CO 2 reformation, oil hydrogenation desulfurization and denitrogenation, F- T synthesis, electro-catalysis water decomposition etc.
Catalytic reaction.
The preparation method of molybdenum carbide mainly has temperature-programmed reaction method, carbothermic method, metallic precursor cracking process at present
Deng.But there are some shortcomings in these existing synthetic methods：As used dangerous fuel gas (CH under high temperature4/H2Or C2H4/H2) institute
Cause operational danger is high, preparation technology is complicated and time-consuming, body of heater needs hyperthermia induced needed for long-time maintenance reaction to ask energy consumption height etc.
Topic.Therefore the strategy for developing simple, the time-consuming synthesis molybdenum carbide catalysis material short, energy consumption is low of a kind of green, safety, technique has
Significance and broad prospect of application.
The content of the invention
In order to overcome the deficiencies in the prior art, quickly prepare carbon it is an object of the present invention to provide a kind of heating of microwave and bear
The method for carrying molybdenum carbide, wherein carrier carbon include：The carbon materials such as CNT, graphene, carbon black, carbon fiber, this method have
Applicability is extensive, green, technique is simple and safety, it is time-consuming it is short, energy consumption is low, is easy to the features such as large-scale production.By this
Method prepare carbon load molybdenum carbide uniform particle sizes it is controllable, crystallinity is high, stability is good.
In order to realize foregoing invention purpose, solve the problems of in the prior art, the technical scheme that the present invention takes
It is：A kind of quick method for preparing carbon load molybdenum carbide of microwave heating, comprises the following steps：
The preparation of step 1, presoma
(a) 10~50mL deionized waters are taken, add 0.2~10g molybdenum salt, 2~30min are stirred, then by 0.2~5g powder
Carbon material is added in solution, continues 2~30min of stirring, after 2~30min of ultrasound, then by obtained dispersion liquid at 40~150 DEG C
Under the conditions of dry, obtain carbon load molybdenum carbide presoma；
(b) 10~50mL deionized waters are taken, add 0.2~10g molybdenum salt, 2~30min is stirred, then carries monoblock type carbon
Body is impregnated into molybdenum salting liquid, stirs 2~20min, after 2~20min of ultrasound, then monoblock type carbon carrier is taken out, 40~150
Dried under the conditions of DEG C, obtain monoblock type carbon load molybdenum carbide presoma；
The one kind of molybdenum salt in ammonium heptamolybdate or sodium molybdate in the step 1, the powder carbon material be selected from carbon black,
One kind in CNT or graphene, the monoblock type carbon carrier are selected from carbon fiber paper；
Step 2, microwave radiation processing
(a) the carbon load molybdenum carbide presoma that step 1 obtains is transferred in microwave reactor, in inert gas shielding
Under, microwave irradiation power control is controlled in 5~1500s in 500~2000W, microwave irradiation time, obtains carbon load carbonization molybdenum materials
Material；
(b) the monoblock type carbon load molybdenum carbide presoma that step 1 obtains is mixed with powder carbon material, then will be mixed
Compound is transferred in microwave reactor, and under inert gas shielding, microwave irradiation power is controlled in 500~2000W, microwave radiation
Then time control is separated the powder carbon material in mixture in 5~1500s, obtain monoblock type carbon load molybdenum carbide
Material；
The one kind of inert gas in nitrogen or argon gas in the step 2, the powder carbon material are selected from graphene
Or one kind in graphite.
Present invention has the advantages that：A kind of quick method for preparing carbon load molybdenum carbide of microwave heating, comprises the following steps：
(1) preparation of presoma, (2) microwave radiation processing.Compared with the prior art, the carbon prepared by this method loads molybdenum carbide grain
Footpath uniform, controllable, crystallinity are high, stability is good.With applicability is extensive, green, technique is simple and safe, takes short, energy
Consume it is low, be easy to the advantages that large-scale production.
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo figure of the carbon black loadings molybdenum carbide prepared in embodiment 1.
Fig. 2 is the X-ray diffraction analysis figure of the carbon nanotube loaded molybdenum carbide prepared in embodiment 2.
Fig. 3 is the stereoscan photograph figure of the carbon fiber loaded molybdenum carbide prepared in embodiment 3.
Fig. 4 is the transmission electron microscope photo figure of the carbon black loadings molybdenum carbide prepared in embodiment 5.
Fig. 5 is the X-ray diffraction analysis figure of the carbon fiber loaded molybdenum carbide prepared in embodiment 6.
Fig. 6 is the X-ray diffraction analysis figure of the carbon black loadings molybdenum carbide prepared in embodiment 8.
Fig. 7 is the stereoscan photograph figure of the carbon fiber loaded molybdenum carbide prepared in embodiment 9.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
20mL deionized waters are taken, add 0.22g ammonium heptamolybdates, stir 10min, then add 0.50g carbon blacks in solution,
5min is stirred, after ultrasonic 10min, then obtained dispersion liquid is dried under the conditions of 80 DEG C, obtains conductive black load molybdenum salt
Compound.Transfer them in microwave reactor, be passed through nitrogen as protection gas, microwave radiation is carried out under 1000W power
After 360s, carbon black loadings carbonization Mo is obtained.From transmission electron microscope picture (Fig. 1) as can be seen that molybdenum carbide (black particle) is equal
Even is distributed on conductive black, and the particle size of particle diameter distribution statistical result showed molybdenum carbide is in 12nm or so.
Embodiment 2
50mL deionized waters are taken, add 1.46g ammonium heptamolybdates, stir 20min, are then added 5.00g CNTs molten
In liquid, 10min is stirred, after ultrasonic 20min, then obtained dispersion liquid is dried under the conditions of 100 DEG C, obtained carbon nanotube loaded
The compound of molybdenum salt.Transfer them in microwave reactor, be passed through argon gas as protection gas, microwave is carried out under 1300W power
After radiating 540s, carbon nanotube loaded carbonization Mo is obtained.From XRD spectra (Fig. 2) as can be seen that carbon nanotube loaded carbon
Change molybdenum free from admixture peak, show that molybdenum carbide purity is high and better crystallinity degree, molybdenum carbide is flat in the material calculated according to Scherrer formula
Equal crystallite dimension is 15nm.
Embodiment 3
25mL deionized waters are taken, add 5.00g ammonium heptamolybdates, 20min is stirred, it is molten that carbon fiber paper is then impregnated into molybdenum salt
In liquid, after stirring 5min, ultrasonic 20min, then carbon fiber paper is taken out and dried under the conditions of 90 DEG C, obtain carbon fiber paper load molybdenum
The compound of salt.It is mixed with graphene, mixture is transferred in microwave reactor afterwards, is passed through argon gas as guarantor
Gas is protected, microwave radiation 600s is carried out under 800W power, after graphene is separated, obtains carbon fiber paper load carbonization Mo.
From scanning electron microscopic picture (Fig. 3) it can be seen that molybdenum carbide particles are uniformly supported on carbon fiber, according to the grain of molybdenum carbide in figure
Footpath distribution statisticses result show that molybdenum carbide Size Distribution is concentrated mainly on 1000nm or so.
Embodiment 4
25mL deionized waters are taken, add 0.38g sodium molybdates, stir 10min, then add 0.60g graphenes in solution,
After stirring 5min, ultrasonic 15min, obtained dispersion liquid is dried under the conditions of 60 DEG C, obtains the compound of graphene-supported molybdenum salt
Thing.Transfer them in microwave reactor, be passed through argon gas and be used as protection gas, after carrying out microwave radiation 300s under 1300W power,
Obtain graphene-supported carbonization Mo.
Embodiment 5
50mL deionized waters are taken, add 0.65g ammonium heptamolybdates, stir 20min, then add 1.50g carbon blacks in solution,
After stirring 5min, ultrasonic 30min, obtained dispersion liquid is dried under the conditions of 120 DEG C, obtains the compound of carbon black loadings molybdenum salt
Thing.Transfer them in microwave reactor, be passed through argon gas and be used as protection gas, after carrying out microwave radiation 500s under 1000W power,
Obtain carbon black loadings carbonization Mo.From transmission electron microscope picture (Fig. 4) it can be seen that molybdenum carbide particles size is in 5~10nm, tool
There is obvious lattice fringe, show higher crystallinity.
Embodiment 6
20mL deionized waters are taken, add 1.25g ammonium heptamolybdates, 20min is stirred, it is molten that carbon fiber paper is then impregnated into molybdenum salt
In liquid, after stirring 15min, ultrasonic 20min, carbon fiber paper is taken out and dried under the conditions of 80 DEG C, obtain carbon fiber paper load molybdenum
The compound of salt.Then it is mixed with graphite powder, mixture is transferred in microwave reactor afterwards, be passed through argon gas work
To protect gas, microwave radiation 600s is carried out under 1000W power, after graphite powder is separated, obtains carbon fiber paper load molybdenum carbide
Material.From XRD spectra (Fig. 5) it can be seen that carbon fiber loaded molybdenum carbide crystallinity is high, and there is no the impurity peaks such as molybdenum oxide,
Show that obtained molybdenum carbide is purer.
Embodiment 7
30mL deionized waters are taken, add 0.25g sodium molybdates, stir 20min, 0.68g CNTs are then added into solution
In, after stirring 15min, ultrasonic 30min, obtained dispersion liquid is dried under the conditions of 130 DEG C, obtains carbon nanotube loaded molybdenum salt
Compound.Transfer them in microwave reactor, be passed through argon gas as protection gas, microwave radiation is carried out under 800W power
After 1200s, carbon nanotube loaded carbonization Mo is obtained.
Embodiment 8
50mL deionized waters are taken, add 0.75g ammonium heptamolybdates, stir 30min, then add 1.25g carbon blacks in solution,
15min is stirred, after ultrasonic 20min, then obtained dispersion liquid is dried under the conditions of 80 DEG C, obtains the compound of carbon black loadings molybdenum salt
Thing.Transfer them to again in microwave reactor, be passed through argon gas as protection gas, microwave radiation 480s is carried out under 1000W power
Afterwards, carbon black loadings carbonization Mo is obtained.From XRD spectra (Fig. 6) it can be seen that the molybdenum carbide of conductive black load is with higher
Crystallinity and purity, the average grain size of molybdenum carbide is 17nm in the material calculated according to Scherrer formula.
Embodiment 9
40mL deionized waters are taken, add 0.50g ammonium heptamolybdates, 20min is stirred, it is molten that carbon fiber paper is then impregnated into molybdenum salt
In liquid, after stirring 15min, ultrasonic 20min, carbon fiber paper is taken out and dried under the conditions of 100 DEG C, obtain carbon fiber paper load molybdenum
The compound of salt.Then it is mixed with graphene, mixture is transferred in microwave reactor afterwards, be passed through argon gas work
To protect gas, microwave radiation 10s is carried out under 850W power, after graphene is separated, obtains carbon fiber paper load carbonization molybdenum materials
Material.From scanning electron microscopic picture (Fig. 7) it can be seen that molybdenum carbide particles are smaller and be equably supported on carbon fiber, according in figure
The particle diameter distribution statistical result of molybdenum carbide show that molybdenum carbide Size Distribution is concentrated mainly on 80nm or so.
Claims (1)
- A kind of 1. quick method for preparing carbon load molybdenum carbide of microwave heating, it is characterised in that comprise the following steps：The preparation of step 1, presoma(a) 10~50mL deionized waters are taken, add 0.2~10g molybdenum salt, 2~30min are stirred, then by 0.2~5g powder carbon materials Material is added in solution, continues 2~30min of stirring, after 2~30min of ultrasound, then by obtained dispersion liquid in 40~150 DEG C of conditions Lower drying, obtain carbon load molybdenum carbide presoma；(b) 10~50mL deionized waters are taken, add 0.2~10g molybdenum salt, 2~30min is stirred, then soaks monoblock type carbon carrier Stain stirs 2~20min into molybdenum salting liquid, after 2~20min of ultrasound, then monoblock type carbon carrier is taken out, in 40~150 DEG C of bars Dried under part, obtain monoblock type carbon load molybdenum carbide presoma；The one kind of molybdenum salt in ammonium heptamolybdate or sodium molybdate in the step 1, the powder carbon material is selected from carbon black, carbon is received One kind in mitron or graphene, the monoblock type carbon carrier are selected from carbon fiber paper；Step 2, microwave radiation processing(a) the carbon load molybdenum carbide presoma that step 1 obtains is transferred in microwave reactor, it is micro- under inert gas shielding Wave radiation Power Control is controlled in 5~1500s in 500~2000W, microwave irradiation time, obtains carbon load carbonization Mo；(b) the monoblock type carbon load molybdenum carbide presoma that step 1 obtains is mixed with powder carbon material, then by mixture It is transferred in microwave reactor, under inert gas shielding, microwave irradiation power is controlled in 500~2000W, microwave irradiation time Control in 5~1500s, then separated the powder carbon material in mixture, obtain monoblock type carbon load carbonization Mo；The one kind of inert gas in nitrogen or argon gas in the step 2, the powder carbon material are selected from graphene or stone One kind in ink.
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Cited By (5)
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| CN109647477A (en) * | 2018-11-26 | 2019-04-19 | 大连理工大学 | A kind of fast preparation method and application of the derivative catalyst of high yield MOF |
| CN109759107A (en) * | 2019-03-22 | 2019-05-17 | 湘潭大学 | A kind of composite catalyst and preparation method thereof |
| CN111705378A (en) * | 2020-06-17 | 2020-09-25 | 武汉纺织大学 | Method for rapidly growing transition metal carbide nano-dots on carbon-based carrier by utilizing microwave combustion and application thereof |
| CN113130809A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Composite electrode and preparation method thereof, and quantum dot light-emitting diode |
| CN115403044A (en) * | 2022-09-14 | 2022-11-29 | 中国矿业大学 | Flexible three-dimensional material with molybdenum carbide growing on surface and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109647477A (en) * | 2018-11-26 | 2019-04-19 | 大连理工大学 | A kind of fast preparation method and application of the derivative catalyst of high yield MOF |
| CN109647477B (en) * | 2018-11-26 | 2021-10-22 | 大连理工大学 | Rapid preparation method and application of high-yield MOF (Metal organic framework) derivative catalyst |
| CN109759107A (en) * | 2019-03-22 | 2019-05-17 | 湘潭大学 | A kind of composite catalyst and preparation method thereof |
| CN113130809A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Composite electrode and preparation method thereof, and quantum dot light-emitting diode |
| CN113130809B (en) * | 2019-12-30 | 2022-06-07 | Tcl科技集团股份有限公司 | Composite electrode and preparation method thereof, and quantum dot light-emitting diode |
| CN111705378A (en) * | 2020-06-17 | 2020-09-25 | 武汉纺织大学 | Method for rapidly growing transition metal carbide nano-dots on carbon-based carrier by utilizing microwave combustion and application thereof |
| CN115403044A (en) * | 2022-09-14 | 2022-11-29 | 中国矿业大学 | Flexible three-dimensional material with molybdenum carbide growing on surface and preparation method and application thereof |
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