CN106229519A - A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst - Google Patents
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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Abstract
The present invention relates to a kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst, coal is crushed to more than 200 mesh, calcining 1～3 hour in 500～1050 DEG C under ammonia and inert gas atmosphere, in the process, programming rate controls at 2～10 DEG C/min；Air velocity is 50～200sccm, and at noble gas or ammonia and the mixed gas protected lower Temperature fall of noble gas, the product taken out in reactor is auto-dope hydrogen reduction and hydrolysis analysis oxygen difunctional oxygen reaction electrocatalysis material.Advantage is: considerably reduce the problem polluting environment that tradition coal resources bring in burning obtains energy process, and success simply utilizes one-step method that low value coal is carried out deep processing to improve its added value, it is prepared for can be used for the auto-dope oxygen reaction electrocatalysis material of the green battery of new forms of energy conversion storage system.
Description
Technical field
The invention belongs to the oxygen reaction electrocatalysis material field of new forms of energy battery, particularly relate to one and utilize coal preparation certainly
The method of the difunctional oxygen that adulterates reaction eelctro-catalyst.
Background technology
Terrestrial climate and city environmental pollution are become to affect with the waste gas that discharged of vehicle that oil product is power source
Main source, energy shortage problem in addition is severeer.Accordingly, it is capable to source and environmental problem have become orthodox car development
Biggest obstacle, finding and developing " low-carbon green new forms of energy " becomes the important content of human civilization in this century.Along with new forms of energy electricity
The rise of pond automobile, operating efficiency and its cost of reduction of improving all kinds of green battery further are Related Research Domain in this century
One of important content.Want finally can commercialization realize big production, find and develop the most cheap non-precious metal and urge
Agent product as an alternative are the most necessary.The research and development that carbon modified composite material is catalysis material of excellent performance provide new contract
Machine.On the other hand, coal is to contain one of big main energy sources of abundant three on the earth, and traditional burning obtains the mode of energy
Causing serious environmental pollution, the eco-friendly high value added utilization therefore improving coal resource is following development trend.
Therefore, that develops that a kind of low value coal utilizing china natural resources abundant prepares high added value can be used for green novel energy source metal-air
The difunctional hydrogen reduction of battery and hydrolysis analysis oxygen eelctro-catalyst are to environment and the sustainable development of the energy and new forms of energy battery
Business application is significant.
Summary of the invention
For overcoming the deficiencies in the prior art, it is an object of the invention to provide one and utilize coal to prepare the difunctional oxygen of auto-dope
The method of reaction eelctro-catalyst, synthetic method is simple, easily operates, and productivity is high, low cost.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of utilize coal prepare auto-dope difunctional oxygen reaction eelctro-catalyst method, coal is crushed to 200 mesh with
On, calcine 1～3 hour in 500～1050 DEG C under ammonia and inert gas atmosphere, in the process, programming rate controls 2
～10 DEG C/min；Air velocity is 50～200sccm, under noble gas or ammonia and noble gas are mixed gas protected
Temperature fall, the product taken out in reactor is auto-dope hydrogen reduction and hydrolysis analysis oxygen difunctional oxygen reaction electrocatalysis material.
Described coal is brown coal, bituminous coal or anthracite.
Described noble gas is nitrogen, argon or helium.
Auto-dope difunctional oxygen reaction eelctro-catalyst include self-doping nitrogen, phosphorus, boron or/and the coal base porous carbon of sulfur, or/
Coal base porous carbon with one or more in auto-dope ferrum, manganese, cobalt, nickel transition metal.
The volume ratio of described ammonia and noble gas mixed gas is 1:10～1:1.
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst, described hydrogen reduction and hydrolysis analysis
Oxygen difunctional oxygen reaction electrocatalysis material mixes with one or more in additional ferrum, cobalt, nickel, manganese transition metal further
Thing is blended, or directly utilizes coal raw material and mix with one or more in additional ferrum, cobalt, nickel, manganese transition metal
Thing is blended, and wherein transition metal and coal base porous charcoal or the raw-material mass ratio of coal are 1:100～1:1, at ammonia and
Under the mixed atmosphere of noble gas at 500～1050 DEG C high-temperature process 1～3 hours；In the process, programming rate controls
2～10 DEG C/min；Air velocity is 20～200sccm；Then protect at noble gas or ammonia and noble gas mixed gas
Protecting lower Temperature fall, the final transition metal Composite Double function oxygen for preparing reacts eelctro-catalyst；Described ammonia and noble gas mix
Volume ratio is 1:10～1:1.
Compared with prior art, the invention has the beneficial effects as follows:
1, the problem polluting environment that tradition coal resources bring in burning obtains energy process is considerably reduced, and
Success simply utilizes one-step method that low value coal is carried out deep processing and improves its added value, is prepared for can be used for new forms of energy conversion
The auto-dope oxygen reaction electrocatalysis material of the green battery of storage system.
2, the auto-dope oxygen reaction electrocatalysis material of the new forms of energy battery of synthesis has good hydrogen reduction and hydrolysis analysis
The starting voltage of oxygen, activity, selectivity and stability.
3, carbon and trace doped element needed for the auto-dope oxygen reaction electrocatalysis material of preparation derive from coal itself.
4, it is blended obtained by coal and one or more mixture in additional ferrum, cobalt, nickel, manganese transition metal
Transition metal Composite Double function oxygen reaction eelctro-catalyst, difunctional hydrogen reduction and the water of electrocatalysis material can be improved further
Resolve the performance of oxygen.
5, synthesis technique is simple, easily operates, and productivity is high, requires the harshest to synthesis device, and low cost can be given birth on a large scale
Produce, it is easy to accomplish industrialization.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscopic picture of original coal in embodiment 1.
Fig. 2 be in embodiment 1 original coal and high temperature ammonia heat treatment later coal base oxygen reaction electrocatalysis material XRD
Figure.
Fig. 3 is the XPS of the coal base oxygen reaction electrocatalysis material that in embodiment 1, original coal high temperature ammonia heat treatment is later
Figure.Wherein black is original coal sample, and red is that the coal base oxygen reaction electricity after direct high temperature processes under ammonia environment is urged
Formed material.
Fig. 4 is the EDX elementary analysis collection of illustrative plates of original coal in embodiment 2.
Fig. 5 is to utilize linear scanning method and the original coal of rotating ring disk electrode (r.r.d.e) detection gained and Ammonia in embodiment 2
The hydrogen reduction linear volt-ampere curve figure of the coal base oxygen reaction electrocatalysis material that gas heat treatment is later.
Fig. 6 be embodiment 3 utilizes linear scanning method and rotating ring disk electrode (r.r.d.e) detection gained high temperature ammonia heat treatment with
After coal base oxygen reaction electrocatalysis material hydrolysis analysis oxygen linear volt-ampere curve figure.
Fig. 7 is the coal base oxygen reaction electro-catalysis utilizing cyclic voltammetry detection high temperature ammonia heat treatment later in embodiment 4
The stability result of material.
Detailed description of the invention
Below in conjunction with Figure of description, the present invention is described in detail, it should be noted that the enforcement of the present invention does not limits
In following embodiment.
The method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst, is crushed to more than 200 mesh by coal,
Calcining 1～3 hour in 500～1050 DEG C under ammonia and inert gas atmosphere, in the process, programming rate controls 2～10
℃/min；Air velocity is 50～200sccm, at noble gas or ammonia and the mixed gas protected lower nature of noble gas
Cooling, the product taken out in reactor is auto-dope hydrogen reduction and hydrolysis analysis oxygen difunctional oxygen reaction electrocatalysis material.
Wherein, coal is brown coal, bituminous coal or anthracite.Noble gas is nitrogen, argon or helium.The difunctional oxygen of auto-dope
Reaction eelctro-catalyst according to the raw-material difference of coal include auto-dope nitrogen, phosphorus, boron or/and the coal base porous carbon of sulfur, or/
One or more the coal base porous carbon in ferrum, manganese, cobalt, nickel transition metal with auto-dope.Ammonia and noble gas mix
The volume ratio closing gas is 1:10～1:1.
Described hydrogen reduction and hydrolysis analysis oxygen difunctional oxygen reaction electrocatalysis material also can further with additional ferrum, cobalt, nickel,
One or more mixture in manganese transition metal are blended, or directly utilize coal raw material and additional ferrum, cobalt, nickel,
One or more mixture in manganese transition metal are blended, metallic element and coal base porous charcoal or the raw-material quality of coal
Than being 1:100～1:1, under the mixed atmosphere of ammonia and noble gas at 500～1050 DEG C high-temperature process 1～3 hours；?
During this, programming rate controls at 2～10 DEG C/min；Air velocity is 20～200sccm；Then at noble gas or
Ammonia and the mixed gas protected lower Temperature fall of noble gas, the final transition metal Composite Double function oxygen for preparing reacts electro-catalysis
Agent；It is 1:10～1:1 that described ammonia and noble gas mix volume ratio.
Embodiment 1
Using Xinjiang brown coal as raw material (shape appearance figure is shown in Fig. 1), grind 5-10 minute in agate mortar so that it is be crushed to
More than 200 mesh, calcining 2 hours under ammonia and argon mixed atmosphere (volume ratio is 1:9) under the conditions of 800 DEG C, reactor exists
After naturally cooling to room temperature under argon shield, take out sample, obtain coal base auto-dope oxygen reaction electrocatalysis material.XRD result table
The bright oxygen that under ammonia environment prepared by high-temperature heat treatment reaction electrocatalysis material contains higher graphite knot compared to original coal
Structure, is shown in Fig. 2, below lines represent original coal sample, above lines be the coal after direct high temperature processes under ammonia environment
Base oxygen reaction electrocatalysis material；XPS result shows the high-temperature heat treatment process that have passed through ammonia environment, oxygen reaction electrocatalysis material
Containing the nitrogen element apparently higher than original coal, see Fig. 3.
Embodiment 2
See Fig. 4 using Inner Mongol brown coal as raw material, EDX elementary analysis, grind 5-10 minute in agate mortar, obtain
The 200 above granules of mesh, calcine 3 hours under ammonia and argon gas atmosphere (volume ratio is 2:8) under the conditions of 700 DEG C, and reactor exists
After naturally cooling to room temperature under argon shield, take out sample, obtain coal base auto-dope oxygen reaction electrocatalysis material.XRD result table
The bright oxygen that under ammonia environment prepared by high-temperature heat treatment reaction electrocatalysis material contains higher graphite knot compared to original coal
Structure；Electrochemical results surface this oxygen reaction electrocatalysis material has fine hydrogen reduction starting voltage, activity and selectivity, sees figure
5, upper graph is original coal sample, and lower surface curve is the coal base oxygen reaction electricity after direct high temperature processes under ammonia environment
Catalysis material.
Embodiment 3
Using Shanxi anthracite as raw material, grinding 5-10 minute in agate mortar, obtaining granularity is more than 200 mesh
Granule, calcines 2 hours under ammonia and argon mixed atmosphere (volume ratio is 1:9) under the conditions of 900 DEG C, and reactor is at inertia argon
After naturally cooling to room temperature under gas shielded, take out sample, obtain coal base auto-dope oxygen reaction electrocatalysis material.Electro-chemical test is tied
Really this oxygen of surface reaction electrocatalysis material has preferably hydrolysis analysis oxygen starting voltage and activity, sees Fig. 6.
Embodiment 4
Using Liaoning bituminous coal as raw material, grind 5-10 minute in agate mortar, at ammonia and argon mixed atmosphere (body
Long-pending than being 3:7) under calcine 2 hours under the conditions of 900 DEG C, after reactor naturally cools to room temperature under inert argon is protected, take
Go out sample, obtain coal base auto-dope oxygen reaction electrocatalysis material.Electrochemical results surface this oxygen reaction electrocatalysis material has
Preferably hydrogen reduction and hydrolysis analysis oxidative stability, be shown in Fig. 7, and solid line is initial cycles voltammogram, when dotted line is scan cycle 1000 times
Cyclic voltammogram (scanning speed is 100mV/s).
Embodiment 5
Using Guizhou anthracite as raw material, grind 5-10 minute in agate mortar, at ammonia and argon mixed atmosphere
Calcining 2 hours under the conditions of 1050 DEG C under (volume ratio is 1:4), reactor naturally cools to room temperature under inert argon is protected
After, take out sample, obtain coal base auto-dope oxygen reaction electrocatalysis material.Subsequently sample is uniformly mixed with cobalt acetate saline solution
(in cobaltous acetate, the weight of cobalt accounts for the 50% of sample), is dried 3 hours in the vacuum drying oven under the conditions of 60 DEG C；Put into logical afterwards
Enter ammonia and the horizontal-type high temperature reacting furnace of argon mixed gas (air velocity is 100sccm, and volume ratio is 1:4), with 5 DEG C/min
Programming rate be heated to 800 DEG C, and continue 2 hours, relief sample under conditions of argon shield, naturally cool to room
Temperature, i.e. obtains the coal-based carbon catalysis material that transition metals cobalt is compound.Wherein, the quality of cobalt element and anthracitic mass ratio are 1:
10。
Embodiment 6
Using Sichuan anthracite as raw material, grind 5-10 minute in agate mortar, obtain the 200 above granules of mesh, with
Afterwards coal sample being mixed with ferric acetate saline solution (in ferric acetate, the weight of ferrum accounts for the 1% of sample), the vacuum under the conditions of 60 DEG C is done
It is dried 2 hours in dry case；Put into afterwards and be passed through ammonia and argon mixed gas (air velocity is 100sccm, and volume ratio is 1:9)
Horizontal-type high temperature reacting furnace, be heated to 800 DEG C with the programming rate of 2 DEG C/min, and continue 3 hours, relief sample at argon
Naturally cool to room temperature under conditions of gas shielded, i.e. obtain the coal-based carbon catalysis material that transition metal iron is compound.
Claims (6)
1. one kind utilizes the method that auto-dope difunctional oxygen reaction eelctro-catalyst prepared by coal, it is characterised in that pulverized by coal
More than 200 mesh, calcining 1～3 hour in 500～1050 DEG C under ammonia and inert gas atmosphere, in the process, heat up speed
Degree controls at 2～10 DEG C/min；Air velocity is 50～200sccm, at noble gas or ammonia and noble gas gaseous mixture
The lower Temperature fall of body protection, the product taken out in reactor is auto-dope hydrogen reduction and hydrolysis analysis oxygen difunctional oxygen reaction electricity is urged
Formed material.
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst the most according to claim 1, its
Being characterised by, described coal is brown coal, bituminous coal or anthracite.
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst the most according to claim 1, its
Being characterised by, described noble gas is nitrogen, argon or helium.
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst the most according to claim 1, its
Be characterised by, auto-dope difunctional oxygen reaction eelctro-catalyst include self-doping nitrogen, phosphorus, boron or/and the coal base porous carbon of sulfur, or/
Coal base porous carbon with one or more in auto-dope ferrum, manganese, cobalt, nickel transition metal.
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst the most according to claim 1, its
Being characterised by, the volume ratio of described ammonia and noble gas mixed gas is 1:10～1:1.
A kind of method utilizing coal to prepare auto-dope difunctional oxygen reaction eelctro-catalyst the most according to claim 1, its
Be characterised by, described hydrogen reduction and hydrolysis analysis oxygen difunctional oxygen reaction electrocatalysis material further with additional ferrum, cobalt, nickel, manganese
One or more mixture in transition metal are blended, or directly utilize coal raw material and additional ferrum, cobalt, nickel, manganese
One or more mixture in transition metal are blended, wherein transition metal and coal base porous charcoal or coal raw material
Mass ratio be 1:100～1:1, under the mixed atmosphere of ammonia and noble gas at 500～1050 DEG C high-temperature process 1～3
Hour；In the process, programming rate controls at 2～10 DEG C/min；Air velocity is 20～200sccm；Then at indifferent gas
Body or ammonia and the mixed gas protected lower Temperature fall of noble gas, final prepare the reaction of transition metal Composite Double function oxygen
Eelctro-catalyst；It is 1:10～1:1 that described ammonia and noble gas mix volume ratio.
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| CN109301246A (en) * | 2018-09-28 | 2019-02-01 | 东北大学秦皇岛分校 | A kind of sulfur doping hard carbon material, preparation method and its kalium ion battery as cathode |
| CN110061199A (en) * | 2018-01-19 | 2019-07-26 | 湖南晋烨高科股份有限公司 | A kind of composite negative pole material of metal-carbon and its preparation method and application |
| CN110479338A (en) * | 2019-09-06 | 2019-11-22 | 新疆大学 | A kind of elctro-catalyst and the preparation method and application thereof |
| CN110943232A (en) * | 2019-12-26 | 2020-03-31 | 辽宁科技大学 | Preparation method of metal air battery electrocatalyst based on coal self-growing carbon nano tube |
| CN111082079A (en) * | 2019-12-30 | 2020-04-28 | 上海交通大学 | Bifunctional oxygen electrocatalyst material and preparation method and application thereof |
| CN111490259A (en) * | 2019-01-25 | 2020-08-04 | 苏州沃泰丰能电池科技有限公司 | Nitrogen-doped and defect-containing porous carbon pore channel loaded cobalt cluster material for zinc-air battery and preparation method thereof |
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| CN111490259A (en) * | 2019-01-25 | 2020-08-04 | 苏州沃泰丰能电池科技有限公司 | Nitrogen-doped and defect-containing porous carbon pore channel loaded cobalt cluster material for zinc-air battery and preparation method thereof |
| CN111490259B (en) * | 2019-01-25 | 2022-05-31 | 苏州沃泰丰能电池科技有限公司 | Nitrogen-doped and defect-containing porous carbon pore channel loaded cobalt cluster material for zinc-air battery and preparation method thereof |
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| CN110943232A (en) * | 2019-12-26 | 2020-03-31 | 辽宁科技大学 | Preparation method of metal air battery electrocatalyst based on coal self-growing carbon nano tube |
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| CN111082079A (en) * | 2019-12-30 | 2020-04-28 | 上海交通大学 | Bifunctional oxygen electrocatalyst material and preparation method and application thereof |
| CN112892549A (en) * | 2021-01-25 | 2021-06-04 | 天津大学 | Catalyst for treating sewage by electrocatalytic oxidation and preparation method thereof |
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