CN105990569B - The preparation method and powder body material of a kind of sulphur carbon composite powder material and application - Google Patents
The preparation method and powder body material of a kind of sulphur carbon composite powder material and application Download PDFInfo
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- CN105990569B CN105990569B CN201510080480.1A CN201510080480A CN105990569B CN 105990569 B CN105990569 B CN 105990569B CN 201510080480 A CN201510080480 A CN 201510080480A CN 105990569 B CN105990569 B CN 105990569B
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Abstract
The present invention provides a kind of preparation method of high-performance sulphur carbon composite powder material, the specific steps are:1, the powder body material of carbon is placed in fluid bed, gas is continually fed into from fluidized-bed bottom, adjusting gas flow rate makes carbon dust be in fluidized state;2, liquid sulfur is made in elemental sulfur, keeps the temperature of liquid sulfur at 113-440 DEG C, liquid sulfur is atomized, by the liquid sulfur penetrating fluid bed of atomization, the powder body material of the liquid sulfur of atomization and the carbon of fluidisation contacts with each other, and sulphur carbon composite powder material is made after cooling." sulphur/carbon " of sulphur carbon composite produced by the present invention than and grain size it is adjustable controllable, composite material carbon and sulphur are evenly distributed, the uniform particle diameter of material;The combination of sulphur and carbon is fine and close in composite material, and conductivity is high;The carbon of sulphur external sheath can effectively inhibit the loss by dissolution and shuttle effect of polysulfide;Composite powder material has spherical or spherical pattern and higher tap density, improves the processing performance of material.
Description
Technical field
The invention belongs to field of chemical power source, be related to a kind of preparation method of lithium sulfur battery anode material, more particularly to one
The preparation method of kind high-performance sulphur carbon composite powder material.
Background technology
Demand of the social development to energy storage technology is growing.Lithium-sulfur cell has high theoretical energy density 2600Wh/
Kg, battery raw material rich reserves, it is at low cost the advantages that, have wide application potential, become grinding for high specific energy secondary cell
Study carefully hot spot.
But lithium-sulfur cell there are problems that.First, the ionic conductivity of elemental sulfur and electron conduction are extremely low;Secondly,
The intermediate product polysulfide of discharge process is easily soluble in organic solvent, occurs " shuttle effect ", leads to loss and the metal of sulphur
The corrosion of lithium ultimately causes battery capacity decaying and service life reduction.In addition, electric discharge final product Li2S or Li2S2Electrical insulating property,
The volume expansion before and after charge and discharge of insoluble and elemental sulfur also results in cycle performance of battery variation.
It is the effective hand for improving lithium sulfur battery anode material conductivity, inhibiting " shuttle effect " to prepare sulphur carbon composite
Section.The method of preparation includes ball milling mixing method, sulphur sublimed method, sulphur dissolution method etc..Material sulphur, carbon made from ball-milling method are unevenly distributed
It is even.The practical loading that the sulphur of material is made in sulphur sublimed method is relatively low.The most of organic solvent used in sulphur dissolution method has poison
Property, it pollutes the environment.
Therefore, it is higher than with material granule size tunable, high efficiency composition, sphericity that there is an urgent need for exploitations a kind of " sulphur/carbon ", and without dirt
Dye, the preparation method of inexpensive, simple for process, favorable reproducibility sulphur carbon composite powder material, to improve the electrochemistry of material
Energy and cyclical stability;And further increase the energy density and cycle life of lithium-sulfur cell.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of high-performance sulphur carbon composite powder material.Prepared by the method
The sulphur carbon ratio of sulphur carbon composite powder material is controllable, powder body material sphericity is high, size tunable.Preparation process is simple, it is at low cost,
Homogeneity of product is high, environmental-friendly, is suitble to large-scale production.
The present invention provides a kind of preparation methods of high-performance sulphur carbon composite powder material, which is characterized in that is made first
Liquid sulfur is atomized by liquid sulfur in high temperature, is contacted with each other with the powder body material of the carbon of fluidisation, chilling be made " sulphur/carbon " ratio and
Grain size is adjustable controllable composite powder material;Specifically comprise the steps of:
Step 1:The powder body material of carbon is placed in fluid bed, gas is continually fed into from fluidized-bed bottom, adjusts gas stream
Speed makes carbon dust be in fluidized state;
Step 2:Liquid sulfur is made in elemental sulfur, keeps the temperature of liquid sulfur at 113-440 DEG C, liquid sulfur is atomized, it will
The powder body material of the liquid sulfur penetrating fluid bed of atomization, the liquid sulfur of atomization and the carbon of fluidisation contacts with each other, and it is compound that sulphur carbon is made
Powder body material.
Spraying stops, and fluidized-bed bottom ventilation stops, and carries out discharging.
The mass ratio of the powder body material of used elemental sulfur and carbon is 1:9–9:1;The grain size D of the powder body material of carbon50For
0.01-10μm。
The elemental sulfur is refined sulphur, sublimed sulfur or one kind in sedimentation sulphur or two kinds or three kinds;The powder of the carbon
Body material be hard carbon or soft carbon or graphite one kind or two kinds or three kinds, the pattern of the powder body material of carbon is graininess, spherical, fine
Tie up the one or two or more kinds of shape, tubulose, sheet or foam-like.
Elemental sulfur is made by liquid sulfur using heat melting method, the heating temperature of heat fusing is 113-440 DEG C, in nitrogen or argon
It is carried out in gas atmosphere.
In step 1, gases used is one or both of nitrogen or argon gas, and the temperature of gas is -30-100 DEG C;Gas
Flow velocity is 0.1m/s-120m/s.
In step 2, when using air-blast atomization, need to use atomization gas, atomizing gas in atomization to be nitrogen or argon
One or both of gas;Mass ratio between the liquid sulfur and atomization gas of atomization is 1:20-100:1;The air-flow of atomization gas
Atomizing pressure is 0.1-10MPa;The nozzle of atomizer is 1-20m at a distance from fluid bed, and the liquid sulfur of atomization is sprayed from atomizer
The rate that mouth sprays is 0.1-120m/s, the grain size D of the liquid sulfur of atomization50It is 0.01-30 μm.
Sulphur carbon composite powder material obtained according to the method described above, the mass ratio of sulphur and carbon is in carbon sulphur composite powder material
1:9–9:1, the grain size D of solid sulfur in material50It is 0.02-30 μm.
Sulphur carbon composite powder material obtained is applied to the positive electrode of lithium-sulfur rechargeable battery according to the method described above.
The present invention can be synthesized using equipment as shown in Figure 1, and synthesis device includes liquid sulfur supply system, atomization
Device, fluid bed, compressed gas supply system and fluidizing gas supply system.
The fluid reservoir in liquid sulfur supply system, feed pump, atomizer, heater, heat indicator in synthesis, and
Pipeline sealing between it, and it is provided with attemperator.
Compressed gas supply system in synthesis device includes gas compressor a, heater, flowmeter, pressure gauge, temperature
Indicating gage, pipeline, and good airproof performance.
Fluidizing gas supply system in synthesis device includes gas compressor b, heater, flowmeter, pressure gauge, temperature
Indicating gage, pipeline, and good airproof performance.
Liquid sulfur fluid reservoir, feed pump, atomizer and the pipeline sealing between it, and it is furnished with heating device, heating temperature
110-440 DEG C of degree;
The present invention has the following advantages:
(1) " sulphur/carbon " of sulphur carbon composite produced by the present invention is adjustable more controllable than with grain size, carbon and sulphur in composite material
Be evenly distributed, the uniform particle diameter of material.
(2) carbon sulphur composite material sulphur and carbon produced by the present invention combine fine and close, and conductivity is high.
(3) carbon sulphur composite material produced by the present invention, the carbon of sulphur external sheath can effectively inhibit the dissolving stream of polysulfide
It becomes estranged shuttle effect.
(4) the sulphur carbon composite powder material that the present invention prepares has spherical or spherical pattern, and tap density is high, improves
The processing performances of electrode plates.
(5) present invention uses totally-enclosed equipment, and preparation process whole process is pollution-free, environmental-friendly.
(6) the adjustable controllable, process of technological parameter of the invention is simply, operation is easy, at low cost, homogeneity of product is high, fits
Close large-scale production.
Therefore, technical scheme of the present invention has controllable Parameter adjustable, technique and is simple to operate and friendly to environment, is at low cost
The advantages of, the composition of obtained sulphur carbon composite is controllable, adjustable, and conductivity is high, and there is spherical morphology, uniform particle diameter to shake
Real density is high, and pole piece processing performance is good, is suitable for the high performance electrode material of lithium-sulfur cell sulphur anode.
The present invention is by atomized liquid sulphur, the powder body material of fluidisation carbon, by spraying atomized liquid sulphur, using between the two
Collision, strong interaction, sulphur carbon composite is directly made.It can regulate and control the ruler of atomized sulfur droplets by controlling atomization parameter
It is very little, and then regulate and control the size of sulphur in composite material;Again by controlling the grain size of toner body material, it is compound that final sulphur carbon can be regulated and controled
" sulphur/carbon " of material compares and the grain size of composite powder material.Therefore, there is material sulphur, carbon composition to be evenly distributed and material particle size
Uniform advantage.Meanwhile in composite material obtained, sulphur and carbon combine densification, are conducive to electron-transport, improve the electricity of composite material
Conductance and tap density;Also, the carbon of sulphur external sheath can also effectively inhibit the loss by dissolution and shuttle effect of polysulfide.Compared with
High tap density and spherical morphology also improves the processing performance of the electrode plates of material.
Description of the drawings
The equipment and process schematic of the preparation method of Fig. 1 sulphur carbon composite powder materials.
1 fluid reservoir, 2 feed pumps, 3 atomizers, 4 fluid beds, 5 gas compressor a, 6 heaters, 7 flowmeters, 8 gas pressures
Contracting machine b, 9 heaters, 10 flowmeters.
Specific implementation mode
The specific implementation mode of the present invention is further described with reference to the accompanying drawings and examples, but is not to be regarded as
Limitation to protection scope of the present invention.
It is carried out in the following example device shown in Fig. 1, the fluid reservoir in liquid sulfur supply system, charging in device
Pump, atomizer, heater and the pipeline sealing between it, and it is provided with attemperator, attemperator presses following implementation respectively
Thermostat temperature setting in example.
Embodiment 1:
Step 1:Under room temperature, 30kg is refined into sulphur and is added in the liquid sulfur supply system of synthesis device, nitrogen is passed through,
115 DEG C by sulphur heat fusing to liquid, and 115 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 30kg grain sizes D50The about graphene powder of 2.6m is added in fluid bed;
Step 3:Start gas compressor, compressed nitrogen enters from fluidized-bed bottom, adjusts gas flow rate about 0.5m/s, makes
Graphene powder is in fluidized state, and the temperature of nitrogen is -30 DEG C;Step 4:Liquid sulfur in fluid reservoir is delivered to atomization chamber
In and be passed through nitrogen, the mass ratio of sulphur and nitrogen is 1:1, the aerodynamic atomization pressure of nitrogen is 0.2MPa, by the liquid sulfur of atomization
It is sprayed into fluid bed with flow velocity about 2m/s;The distance of atomizer nozzle to fluid bed is 10m, and heating devices heat temperature is 115
℃;The atomizing particle size D of liquid sulfur50About 0.1 μm;
" sulphur/graphene " composite material is made, the grain size D of sulphur ball in material50About 20m, " sulphur/carbon " mass ratio about 1:1.
Embodiment 2:
Step 1:Under room temperature, 1kg sedimentation sulphur is added in the liquid sulfur supply system of synthesis device.It is passed through nitrogen,
200 DEG C by sulphur heat fusing to liquid, and 200 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 9kg grain sizes D50About 0.01m simultaneously there are the carbon black powders of meso-hole structure to be added in fluid bed;
Step 3:Starting gas compressor, compressed nitrogen enters from fluidized-bed bottom, and it is about 100m/s to adjust gas flow rate,
Carbon dust is set to be in fluidized state, 100 DEG C of the temperature of nitrogen;
Step 4:Liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, the mass ratio of sulphur and nitrogen is 1:
10, the aerodynamic atomization pressure of nitrogen is 10MPa, by the liquid sulfur of atomization with flow velocity about 120m/s, atomizer nozzle to fluid bed
Distance be 2m;Heating devices heat temperature is 200 DEG C;The atomizing particle size D of liquid sulfur50About 0.005 μm;
" sulphur/carbon black " composite material is made, the grain size D of sulphur in material50About 0.02m, " sulphur/carbon " mass ratio about 1:9.
Embodiment 3:
Step 1:Under room temperature, 81kg sublimed sulfurs are added in the liquid sulfur supply system of synthesis device.It is passed through argon gas,
440 DEG C by sulphur heat fusing to liquid, and 440 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 9kg grain sizes D50The about carbon nanotube of 0.5m is added in the fluid bed of synthesis device;
Step 3:Starting gas compressor, compressed argon enters from fluidized-bed bottom, and it is about 0.1m/s to adjust gas flow rate,
Carbon nanotube dust is set to be in fluidized state, the temperature of argon gas is -10 DEG C;
Step 4:Liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through argon gas, the mass ratio 8 of sulphur and argon gas:2,
The aerodynamic atomization pressure of argon gas is 0.1MPa, the liquid sulfur of atomization is sprayed into flow velocity about 0.8m/s in fluid bed, atomizer spray
The distance of mouth to fluid bed is 20m;Heating device temperature is 440 DEG C;The atomizing particle size D of liquid sulfur50About 0.5 μm;
" sulphur/carbon nanotube " composite material is made, the grain size D of sulphur ball in material50About 30m, " sulphur/carbon " mass ratio about 9:
1。
Embodiment 4:
Step 1:Under room temperature, 4kg sublimed sulfurs are added in the liquid sulfur supply system of synthesis device.It is passed through argon gas,
180 DEG C by sulphur heat fusing to liquid, and 180 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 16kg grain sizes D50The carbon fiber powder of about 10m is added in the fluid bed of synthesis device;
Step 3:Starting gas compressor, compressed argon enters from fluidized-bed bottom, and it is about 0.5m/s to adjust gas flow rate,
Carbon fiber powder is set to be in fluidized state, the temperature of argon gas is 0 DEG C;
Step 4:Liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through argon gas, the mass ratio of sulphur and argon gas is 4:
6, the aerodynamic atomization pressure of argon gas is 0.12MPa, and the liquid sulfur of atomization is sprayed into flow velocity about 1m/s in fluid bed;Heating device
Temperature is 180 DEG C;The atomizing particle size D of liquid sulfur50About 0.25 μm;
" sulphur/carbon fiber " composite material is made, the grain size of sulphur ball is about 28m, " sulphur/carbon " mass ratio about 1 in material:4.
Embodiment 5:
Step 1:Under room temperature, 9kg sublimed sulfurs are added in the liquid sulfur supply system of synthesis device.It is passed through nitrogen,
150 DEG C by sulphur heat fusing to liquid, and 150 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 6kg grain sizes D50The foam toner body of about 0.01m is added in the fluid bed of synthesis device;
Step 3:Start gas compressor, compressed nitrogen enters from fluidized-bed bottom, adjusts gas flow rate about 15m/s, makes
Foam toner body is in fluidized state, and the temperature of nitrogen is 25 DEG C;
Step 4:Liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, the mass ratio of sulphur and nitrogen is 6:
4, the aerodynamic atomization pressure of nitrogen is 4MPa, the liquid sulfur of atomization is sprayed into flow velocity about 50m/s in fluid bed, atomizer nozzle
Distance to fluid bed is 5m;Heating device temperature is 150 DEG C;The atomizing particle size D of liquid sulfur50About 0.03 μm;
" sulphur/foamy carbon " composite material is made, the grain size D of sulphur ball in material50About 0.1m, " sulphur/carbon " mass ratio about 3:
2。
Embodiment 6:
Step 1:Under room temperature, 16kg sedimentation sulphur is added in the liquid sulfur supply system of synthesis device.It is passed through argon gas,
300 DEG C by sulphur heat fusing to liquid, and 300 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 24kg grain sizes D50The carbonaceous mesophase spherules powder of about 2m is added in the fluid bed of synthesis device;
Step 3:Start gas compressor, compressed argon enters from fluidized-bed bottom, and it is about 2m/s to adjust gas flow rate, is made
Carbonaceous mesophase spherules powder is in fluidized state, and the temperature of argon gas is 70 DEG C;
Step 4:Liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through argon gas, using air-blast atomization, sulphur with
The mass ratio of argon gas is 3:7, the aerodynamic atomization pressure of argon gas is 0.4MPa, and the liquid sulfur of atomization is sprayed into stream with flow velocity about 5m/s
Change in bed, the distance of atomizer nozzle to fluid bed is 10m;Heating device temperature is 300 DEG C;The atomizing particle size D of liquid sulfur50About
It is 0.1 μm;
" sulphur/carbonaceous mesophase spherules " composite material is made, the grain size D of sulphur ball in material50About 11m, " sulphur/carbon " mass ratio
2:3。
Embodiment 7:
Step 1:Under room temperature, 8kg is refined into sulphur and is added in the liquid sulfur supply system of synthesis device.It is passed through nitrogen,
160 DEG C by sulphur heat fusing to liquid, and 160 DEG C of constant temperature is stored in fluid reservoir;
Step 2:By 2kg grain sizes D50The absorbent charcoal powder body of about 0.6m is added in the fluid bed of synthesis device;
Step 3:Start gas compressor, compressed nitrogen enters from fluidized-bed bottom, and adjusting gas flow rate, which is about 1m/s, to be made
Absorbent charcoal powder body is in fluidized state, and the temperature of nitrogen is 40 DEG C;
Step 4:Liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, the mass ratio of sulphur and nitrogen is 8:
2, the aerodynamic atomization pressure of nitrogen is 0.3MPa, the liquid sulfur of atomization is sprayed into flow velocity about 4m/s in fluid bed, atomizer spray
The distance of mouth to fluid bed is 10m;Heating device temperature is 160 DEG C;The atomizing particle size D of liquid sulfur50About 0.12 μm;
" sulphur/activated carbon " composite material is made, the grain size D of sulphur ball in material50About 15m, " sulphur/carbon " mass ratio 4:1.
Although present disclosure makes specific introduction by above-described embodiment, above-described embodiment should not be considered as
Limitation of the present invention.Therefore, protection scope of the present invention should be defined by the appended claims.
Claims (8)
1. a kind of preparation method of sulphur carbon composite powder material, it is characterised in that:Liquid sulfur is made first, liquid sulfur is atomized,
It contacts with each other with the powder body material of the carbon of fluidisation, " sulphur/carbon " ratio and the regulatable composite powder material of grain size is made;Specific step
Suddenly it is:
Step 1:The powder body material of carbon is placed in fluid bed, gas is continually fed into from fluidized-bed bottom, adjusting gas flow rate makes
Carbon dust is in fluidized state;
Step 2:Liquid sulfur is made in elemental sulfur, keeps the temperature of liquid sulfur in 113-440oLiquid sulfur is atomized by C, by atomization
The powder body material of liquid sulfur penetrating fluid bed, the liquid sulfur of atomization and the carbon of fluidisation contacts with each other, and sulphur carbon composite powder material is made
Material.
2. preparation method according to claim 1, it is characterised in that:The matter of the powder body material of used elemental sulfur and carbon
Amount is than being 1:9 – 9:1;The grain size D of the powder body material of carbon50It is 0.01-10 μm.
3. preparation method according to claim 1, it is characterised in that:The elemental sulfur is refined sulphur, sublimed sulfur or heavy
One kind in sulfur reduction or two kinds or three kinds;The powder body material of the carbon be one kind in hard carbon, soft carbon or graphite or two kinds or
Three kinds, the pattern of the powder body material of carbon be graininess, spherical, fibrous, tubulose, sheet or one kind in foam-like or two kinds with
On.
4. preparation method according to claim 1, it is characterised in that:It is gases used in nitrogen or argon gas in step 1
A kind of or two kinds, the temperature of gas is -30-100oC;Gas flow rate is 0.1m/s-120 m/s.
5. preparation method according to claim 1, it is characterised in that:Elemental sulfur is made by liquid sulfur using heat melting method,
The heating temperature of heat fusing is 113-440oC is carried out in nitrogen or argon gas atmosphere.
6. preparation method according to claim 1 or 5, it is characterised in that:In step 2, atomizing gas is nitrogen or argon
One or both of gas;Mass ratio between the liquid sulfur and atomization gas of atomization is 1:20-100:1;The air-flow of atomization gas
Atomizing pressure is 0.1-10MPa;The grain size D of the liquid sulfur of atomization50It is 0.01-30 μm;The nozzle of atomizer and fluid bed away from
It is 0.1-120 m/s from the rate that the liquid sulfur for 1-20m, atomization is sprayed from atomizer nozzle.
7. sulphur carbon composite powder material made from a kind of the method any according to claim 1-5, it is characterised in that:Carbon sulphur
The mass ratio of sulphur and carbon is 1 in composite powder material:9 – 9:1, the grain size D of solid sulfur in material50It is 0.02-30 μm.
8. sulphur carbon composite powder material the answering in the positive electrode for preparing lithium-sulfur rechargeable battery described in a kind of claim 7
With.
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CN114025874A (en) * | 2019-06-28 | 2022-02-08 | 壹久公司 | Processing system and method with secondary gas flow |
IT201900016178A1 (en) * | 2019-09-12 | 2021-03-12 | Fondazione St Italiano Tecnologia | PROCESS FOR THE PRODUCTION OF A SULFUR-CARBON COMPOSITE MATERIAL, COMPOSITE MATERIAL SO OBTAINED AND ELECTRODE FOR LITHIUM-SULFUR BATTERIES PRODUCED WITH THE MATERIAL |
CN114784261B (en) * | 2022-06-21 | 2022-09-23 | 宜宾锂宝新材料有限公司 | Lithium battery positive electrode material and preparation method thereof |
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