CN107298442A - A kind of biomass carbon/molybdenum disulfide nano-composite material and preparation method thereof - Google Patents
A kind of biomass carbon/molybdenum disulfide nano-composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of biomass carbon/molybdenum disulfide nano-composite material and preparation method thereof.The preparation method of the present invention includes：Biomass carbon is prepared by hydro-thermal method and calcining, petal-shaped molybdenum disulfide nano material is then grown on multiporous biological matter carbon by one step hydro thermal method.The features such as conductive good, electrochemical properties of biomass carbon/molybdenum disulfide nano-composite material prepared by the present invention are stable, can be as a kind of preferable high-performance electric catalyzing manufacturing of hydrogen material, and lubricant, battery material, catalysis material, hydrogen storage material etc..The preparation method of the present invention is simple to operate, with low cost, has a extensive future.
Description
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of biomass carbon/molybdenum disulfide nano composite wood
Material and preparation method thereof.
Background technology
World energy sources structure based on coal and oil causes global environmental pollution and destruction, such as coal burning and vapour
It is complete caused by depletion of the ozone layer that acid rain and haze, chloro-fluoro-carbon kind discharge caused by tail gas discharge are caused, greenhouse gas emission
Ball warms and its derivative Melting Glacierss, the problems such as sea level rise, these none do not endanger people it is healthy even
Survival and development.The environmental problems such as energy crisis and greenhouse effects that the whole world faces are solved, best bet is exactly to develop
Hydrogen Energy.Hydrogen is as a kind of clean type energy, and the product after burning or catalysis oxidation is water, is not polluted the environment not only, also
Can as further hydrogen manufacturing raw material, water electrolysis hydrogen production, recycle.However, conventional alkaline electrolysis process hydrogen production efficiency is low, electricity
It can be lost greatly, application is limited.Although and acidic electrolysis technique efficiency high, heavy dependence noble metal（Pt）Catalyst.Cause
How this, solve the key problem that high hydrogen production efficiency and the low contradiction for being catalyzed cost are electro-catalysis hydrogen manufacturing.
The discovery of graphene causes two-dimensional layer material to flourish, and molybdenum disulfide（MoS2）Also due to it has class stone
Extensive concern of the structure of black alkene by researcher.Nanometer MoS2Marginal texture is complicated, and unsaturation is very high, relatively more active,
There are very big potentiality in catalyst application aspect.At present, MoS2It is widely used as Hydrobon catalyst, because it not only has height
Catalytic activity, moreover it is possible to prevent sulfur poisoning.MoS2There is the lance of electric conductivity, avtive spot and stability when carrying out electro-catalysis hydrogen manufacturing
Shield, therefore, to MoS2Be combined turns into the study hotspot in the field to improve its stability, electric conductivity and catalytic.
Most common property-modifying additive is nanometer carbon material.2013, Liao et al. made MoS by hydro-thermal method2/
Porous oxidation graphene nanocomposite material, with pure MoS2Material is compared, and has shown low hydrogen manufacturing overpotential（η）, it is high
Hydrogen production efficiency and high cyclical stability（Liao L, Zhu J, Bian X, et al., Adv. Funct. Mater.,
2013, 23: 5326.）.2014, Yang et al. prepared MoS2/ absorbent charcoal composite material, equally improves MoS2System
Hydrogen efficiency（Zhao X, Zhu H, Yang X., Nanoscale, 2014, 6(18): 10680-10685.）.However, mesh
The acquisition of the more nano-carbon material of preceding research depends on fossil energy.It is increasingly tight with environmental pollution since 20 end of the centurys
The continuous aggravation of weight and energy crisis, this just forces us to seek the raw material for preparing carbon material more cleaned.
The content of the invention
It is an object of the invention to provide a kind of electrocatalytic hydrogen evolution activity is high, stability is good, with low cost, preparation process is environmentally friendly
Biomass carbon/molybdenum disulfide nano-composite material and preparation method thereof.
The present invention uses maize straw for raw material, multiporous biological matter carbon is made through hydrothermal carbonization and high-temperature activation, in this base
Hydro-thermal method grows petal-like MoS on multiporous biological matter carbon on plinth2, finally obtained electrocatalytic hydrogen evolution activity height, stability are good
Biomass carbon/molybdenum disulfide nano-composite material.
The preparation method of the present invention comprises the following steps：
（1）The preparation of biomass carbon
First maize straw material is pre-processed, then by stalk hydrothermal carbonization, biomass carbon is made in high-temperature activation；
（2）Hydro-thermal method synthesising biological matter carbon/molybdenum disulfide nano-composite material
Using ultra-pure water as solvent, prepare after Ammonium Molybdate Tetrahydrate, the mixed solution of thiocarbamide, stirring and dissolving and step（1）In it is made
Standby biomass carbon is put into reactor together carries out hydro-thermal reaction, then by obtained product suction filtration, deionized water and anhydrous
Ethanol is cleaned, and is dried, is ultimately formed biomass carbon/molybdenum disulfide nano-composite material.
Step（1）Described pretreatment is thoroughly dried again after one week with soaked in absolute ethyl alcohol.
Step（1）Described biomass carbon is porous chips layer structure.
Step（1）The temperature of described hydrothermal carbonization is 100 ~ 200 DEG C, and the time is 12 ~ 50 h.
Step（1）Described high-temperature activation, inert gas used is high pure nitrogen, and the temperature of high-temperature activation is 400 ~ 800
DEG C, the high-temperature activation time is 0.5 ~ 2 h.
Step（2）The concentration of described Ammonium Molybdate Tetrahydrate is that 1 ~ 5 mg/mL, the concentration of thiocarbamide are 2 ~ 8 mg/mL, biological
The mass ratio of matter carbon and Ammonium Molybdate Tetrahydrate is 1:10~1:1.
Step（2）The temperature of described hydro-thermal reaction is 120 ~ 280 DEG C, and the time is 12 ~ 24 h.
Biomass carbon/molybdenum disulfide nano-composite material that above-mentioned preparation method is prepared and described biomass carbon/
Molybdenum disulfide nano-composite material is in fields such as electro-catalysis hydrogen manufacturing material, lubricant, battery material, catalysis material, hydrogen storage materials
Application.
The invention has the advantages that：
（1）Biomass carbon raw material chooses aboundresources, inexpensive, wide material sources agricultural production discarded object-corn stalks, waste profit
With, turn waste into wealth, it is to avoid use fossil energy, realize cleanliness without any pollution, sustainable development；The biomass carbon of preparation,
It is the graphited amorphous carbon material in part, shortrange order, longrange disorder, with good electric conductivity in structure；It is on pattern
A kind of micron order of porous sheet even nanometer materials, specific surface area is big, and high surface is conducive to molybdenum disulfide to exist
The growth on surface.
（2）After being combined with biomass carbon, MoS2The shape of petal is still maintained, edge is relatively thin, specific surface area and activity
Site increases, while electric conductivity is good, improves liberation of hydrogen efficiency；The hydrogen manufacturing of biomass carbon/molybdenum disulfide composite catalyst
Current density may be up to 155 mA cm-2, and the material also shows excellent electro-catalysis stability, is followed by 10000 times
Good catalytic activity is still kept after ring.
（3）The preparation method of the present invention is simple to operate, with low cost, has a extensive future.
Brief description of the drawings
Fig. 1 is the biomass carbon stereoscan photograph prepared by embodiment 1.
Fig. 2 is the biomass carbon transmission electron microscope photo prepared by embodiment 1.
Fig. 3 is biomass carbon/molybdenum disulfide nano-composite material stereoscan photograph prepared by embodiment 1.
Fig. 4 is biomass carbon/molybdenum disulfide nano-composite material transmission electron microscope photo prepared by embodiment 1.
Fig. 5 is that biomass carbon/molybdenum disulfide nano-composite material prepared by embodiment 1 is 200 mV in overpotential
Hydrogen manufacturing stability curve figure.
Fig. 6 is the front and rear hydrogen manufacturing of 2000 circulations of biomass carbon/molybdenum disulfide nano-composite material prepared by embodiment 1
Polarization curve.
Embodiment
Below in conjunction with the accompanying drawings and the present invention will be described in detail by specific embodiment, so that advantages of the present invention and spy
Levying can be easier to be readily appreciated by one skilled in the art, and apparent clearly be defined so as to be made to protection scope of the present invention.
Embodiment 1：
（1）Hydro-thermal method prepares biomass carbon：
It is accurate to weigh 1.5 g pretreatments（Thoroughly dried after soaked in absolute ethyl alcohol pretreatment in one week）The maize straw crossed is in water heating kettle
Liner, adds the 2.5 ml concentrated sulfuric acids and 50 ml ultra-pure waters, is sealed after being well mixed, and the h of hydro-thermal reaction 48 at 180 DEG C is natural
Cooling.
Biomass carbon is collected by filtration, is first cleaned with ultra-pure water 3 times, then is dried with ethanol thoroughly cleaning.
Dry biomass carbon and active material potassium hydroxide（KOH）With mass ratio 1:2 mixing, grind in agate mortar
Uniformly.
The biomass carbon mixed with active material is placed in tube furnace, pre- logical nitrogen（N2）30min eliminates air, starts
Calcining.Using temperature-gradient method, 400 DEG C of holding 30min are first warming up to, then be warming up to 800 DEG C of holding 1h, natural cooling.Heating speed
Rate is 10 DEG C/min.
Biomass carbon sample 2M HCl and ultra-pure water thoroughly cleaning after activation, then cleaned 3 times with ethanol, dry.Grind
Mill collects sample.
Prepared biomass carbon stereoscan photograph is as shown in Figure 1.（a）With（b）It is that being similar to for biomass carbon is macroscopical
Sponge structure.（c）With（d）Multiplication factor is smaller, but is clear that the laminar structured and its uniformity of carbon.As schemed
2 be the TEM figures of the biomass carbon prepared, further shows the lamellar structure and loose structure of biomass carbon, can from figure
It is micron order even nanoscale to its hole and thickness.
（2）Hydro-thermal method prepares biomass carbon/molybdenum disulfide nano-composite material：
Biomass carbon that 0.05g prepares accurately is weighed with electronic analytical balance in water heating kettle, then weighs the hydrations of 0.2418g tetra-
Ammonium molybdate, 0.4567g thiocarbamides are poured into the water heating kettle for fill biomass carbon in beaker, plus after 70ml ultra-pure water stirring and dissolvings and mixed
Close uniform, sealing.
The natural cooling after the h of hydro-thermal reaction 18 at 220 DEG C, suction filtration obtains product, with deionized water and washes of absolute alcohol
After be dried to obtain final products.
Such as Fig. 3 is the SEM pictures of the biomass carbon/molybdenum disulfide composite prepared, as we can see from the figure in biology
One layer of white material of the Surface Creation of matter carbon material, these white materials are exactly MoS2, realize biomass carbon and MoS2
It is compound.Fig. 4 is the TEM pictures of the biomass carbon/molybdenum disulfide composite prepared, apparent can be seen from TEM figures
It is grown in the petal-like MoS on biomass carbon2.After being combined with biomass carbon, MoS2Still keep the petal-shaped of its original, edge
It is relatively thin, it is possible to provide more avtive spots.As shown in figure 5, when overpotential is 200mV after 10000 times circulate, electric current is several
It is constant；As shown in fig. 6, biomass carbon/molybdenum disulfide composite catalyst is in the catalytic activity after 2000 times circulate
It is held essentially constant, this has all absolutely proved the stability of catalyst electrocatalytic hydrogen evolution in acid condition.
Embodiment 2：
（1）Hydro-thermal method prepares biomass carbon：
The accurate pretreated maize straws of 1.5 g that weigh add the 2.5 ml concentrated sulfuric acids and 50 ml are ultrapure in water heating kettle liner
Water, is sealed, the h of hydro-thermal reaction 36, natural cooling at 200 DEG C after being well mixed.
Biomass carbon is collected by filtration, is first cleaned with ultra-pure water 3 times, then is dried with ethanol thoroughly cleaning.
Dry biomass carbon and active material potassium hydroxide（KOH）With mass ratio 1:3 mixing, grind in agate mortar
Uniformly.
The biomass carbon mixed with active material is placed in tube furnace, pre- logical nitrogen（N2）30min eliminates air, starts
Calcining.Using temperature-gradient method, 400 DEG C of holding 30min are first warming up to, then be warming up to 800 DEG C of holding 1h, natural cooling.Heating speed
Rate is 10 DEG C/min.
Biomass carbon sample 2M HCl and ultra-pure water thoroughly cleaning after activation, then cleaned 3 times with ethanol, dry.Grind
Mill collects sample.
（2）Hydro-thermal method prepares biomass carbon/molybdenum disulfide nano-composite material：
Biomass carbon that 0.05g prepares accurately is weighed with electronic analytical balance in water heating kettle, then weighs the hydrations of 0.2418g tetra-
Ammonium molybdate, 0.4567g thiocarbamides are poured into the water heating kettle for fill biomass carbon in beaker, plus after 70ml ultra-pure water stirring and dissolvings and mixed
Close uniform, sealing.
The natural cooling after the h of hydro-thermal reaction 18 at 220 DEG C, suction filtration obtains product, with deionized water and washes of absolute alcohol
After be dried to obtain final products.
Embodiment 3
（1）Hydro-thermal method prepares biomass carbon：
The accurate pretreated maize straws of 1.5 g that weigh add the 2.5 ml concentrated sulfuric acids and 50 ml are ultrapure in water heating kettle liner
Water, is sealed, the h of hydro-thermal reaction 48, natural cooling at 180 DEG C after being well mixed.
Biomass carbon is collected by filtration, is first cleaned with ultra-pure water 3 times, then is dried with ethanol thoroughly cleaning.
Dry biomass carbon and active material potassium hydroxide（KOH）With mass ratio 1:2 mixing, grind in agate mortar
Uniformly.
The biomass carbon mixed with active material is placed in tube furnace, pre- logical nitrogen（N2）30min eliminates air, starts
Calcining.Using temperature-gradient method, 400 DEG C of holding 30min are first warming up to, then be warming up to 800 DEG C of holding 1h, natural cooling.Heating speed
Rate is 10 DEG C/min.
Biomass carbon sample 2M HCl and ultra-pure water thoroughly cleaning after activation, then cleaned 3 times with ethanol, dry.Grind
Mill collects sample.
（2）Hydro-thermal method prepares biomass carbon/molybdenum disulfide nano-composite material：
Biomass carbon that 0.025g prepares accurately is weighed with electronic analytical balance in water heating kettle, then weighs the water of 0.1204g tetra-
Ammonium molybdate is closed, 0.2284g thiocarbamides are poured into the water heating kettle for filling biomass carbon in beaker, plus after 50ml ultra-pure water stirring and dissolvings
It is well mixed, sealing.
The natural cooling after the h of hydro-thermal reaction 18 at 220 DEG C, suction filtration obtains product, with deionized water and washes of absolute alcohol
After be dried to obtain final products.
Claims (9)
1. a kind of preparation method of biomass carbon/molybdenum disulfide nano-composite material, it is characterised in that comprise the following specific steps that：
（1）The preparation of biomass carbon：First maize straw material is pre-processed, then by stalk hydrothermal carbonization, high-temperature activation,
Biomass carbon is made；
（2）Hydro-thermal method synthesising biological matter carbon/molybdenum disulfide nano-composite material：Using ultra-pure water as solvent, four molybdic acid hydrates are prepared
After the mixed solution of ammonium, thiocarbamide, stirring and dissolving and step（1）In prepared biomass carbon be put into reactor enter water-filling together
Thermal response, then by obtained product suction filtration, deionized water and washes of absolute alcohol, dries, ultimately forms the sulphur of biomass carbon/bis-
Change molybdenum nano composite material.
2. preparation method according to claim 1, it is characterised in that step（1）Described pretreatment is soaked with absolute ethyl alcohol
Steep and thoroughly dried again after one week.
3. preparation method according to claim 1, it is characterised in that step（1）Described biomass carbon is porous chips stratiform
Structure.
4. preparation method according to claim 1, it is characterised in that step（1）The temperature of described hydrothermal carbonization is 100
~200 DEG C, the time is 12~50 h.
5. preparation method according to claim 1, it is characterised in that step（1）The indifferent gas that described high-temperature activation is used
Body is high pure nitrogen, and the temperature of high-temperature activation is 400~800 DEG C, and the high-temperature activation time is 0.5~2 h.
6. preparation method according to claim 1, it is characterised in that step（2）The concentration of described Ammonium Molybdate Tetrahydrate is
1~5 mg/mL, the concentration of thiocarbamide are 2~8 mg/mL, and the mass ratio of biomass carbon and Ammonium Molybdate Tetrahydrate is 1:10~1:1.
7. preparation method according to claim 1, it is characterised in that step（2）The temperature of described hydro-thermal reaction is 120
~280 DEG C, the time is 12~24 h.
8. the preparation-obtained biomass carbon/molybdenum disulfide nano-composite material of claim 1~7 any one preparation method.
9. biomass carbon/molybdenum disulfide nano-composite material described in claim 8 as electro-catalysis hydrogen manufacturing material, lubricant,
Battery material, catalysis material, the application of hydrogen storage material.
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| CN108091837A (en) * | 2017-11-24 | 2018-05-29 | 北京欧美中科学技术研究院 | A kind of molybdenum disulfide/carbon composite and its preparation method and application |
| CN108441884A (en) * | 2018-04-24 | 2018-08-24 | 江苏科技大学 | Compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of molybdenum disulfide/carbon and preparation method thereof |
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| CN113247955A (en) * | 2021-05-14 | 2021-08-13 | 同济大学 | Composite material and preparation method and application thereof |
| CN113782713A (en) * | 2021-07-09 | 2021-12-10 | 苏州科技大学 | MoS2Nano-sheet vertically embedded biological carbon nano composite material and preparation method and application thereof |
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| CN115475606A (en) * | 2022-10-19 | 2022-12-16 | 辽宁大学 | Modified molybdenum sulfide/charcoal material, preparation method thereof and application thereof in co-adsorption of antibiotics and heavy metal ions |
| CN116273070A (en) * | 2023-02-27 | 2023-06-23 | 广州大学 | Oleaceae-based biomass bimetallic sulfide catalyst and preparation method and application thereof |
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