CN101800316A - Preparation method of porous carbon cathode material and primary lithium battery using porous carbon cathode material - Google Patents
Preparation method of porous carbon cathode material and primary lithium battery using porous carbon cathode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a porous carbon cathode material and a primary lithium battery using the porous carbon cathode material. The porous carbon cathode material comprises the components such as carbon black, additives and binder. The preparation method comprises the following steps: mixing the raw materials with water, pulping, then dewatering for drying, foaming for pore-forming, and performing vacuum drying and other processes. The material is used as cathode carrier, liquid SOCl2, SO2Cl2, SO2 or other active material is used as cathode active material and metal lithium is used as anode active material to prepare the high-energy-density primary lithium battery. The preparation process of the material uses water as solvent without using ethanol, isopropanol or other flammable organic solvents, thus increasing the safety, improve the working environment, facilitating the mechanized and scale manufacture, reducing the labor intensity and significantly improving the consistency and stability of the electrical characteristics of batteries.
Description
Technical field
The present invention relates to a kind of cathode material of lithium primary cell, relate in particular to a kind of preparation method of cathode materials for lithium battery of liquid cathode active material and the lithium primary cell that uses this material.
Background technology
With the lithium metal is the lithium battery that anode, negative electrode adopt liquid active material, for example lithium/thinly chloride (Li/SOCl
2) battery, lithium/chlorosulfuric acid (Li/SO
2Cl
2) and lithium/sulfur dioxide (Li/SO
2) battery etc., it is the present the highest primary cell of specific energy in the battery system of practical application in the world, liquid active material in the battery need store in the porous carbon negative electrode and react, that is to say that the porous carbon negative electrode is the warehousing storage of liquid active material, it is again the place of liquid active material generation electrochemical reaction, and play catalysis and afflux simultaneously, in the battery of liquid active material, have important status as negative electrode.These porous carbon cathode materials in the lithium battery that can be used for the liquid cathode active material, can also be used for metal-air battery, fuel cell or the like field.In lithium primary cell, its liquid cathode material is normally based on the mixture of carbon black and ptfe emulsion, carbon black uses acetylene black usually, has hydrophobicity, not with water parent profit, but with organic solvent parent profit, so in this cathode material preparation process, use the solvent of inflammable and explosive organic solvent such as alcohol, isopropyl alcohol usually, not environmental protection as mixed process, also very dangerous, also have a strong impact on workman's operating environment.
For example existing lithium/thinly chloride battery cathode material is to be got by the preparation of processes such as batch mixing, moulding, oven dry, foaming, vacuum drying.During batch mixing earlier with acetylene black, as the copper powder of functional additive or other catalytic active substances (for example application number is disclosed metal phthalocyanine/carbon nano tube composite catalyst of application for a patent for invention Publication Specification of 200910038262.6 or the like), as the ethanol (alcohol) of solvent or isopropyl alcohol, ptfe emulsion (mass ratio is 60% emulsion) by 25: 2: 156: 2 mass ratio is got material, join again in the mixture of acetylene black and copper powder after ptfe emulsion and alcohol mixed, obtain mixture after stirring, mixing.Make the negative electrode of different shapes then according to the needs of battery pole piece shaped design.With the oven dry of the negative electrode after the moulding, handle through the high temperature foaming again, obtain the carbon cathode of porous, after vacuum drying is handled, thoroughly remove the moisture in the carbon cathode, promptly obtain needed cathode materials for lithium battery.Because alcohol is a kind of volatile, incendive liquid, in the batch mixing process, the volatile quantity of difficult control alcohol, dangerous high in the manufacturing process, and this technology is not suitable for large-scale production, and labor strength is big, and gained battery product consistency is bad.
Summary of the invention
The technical problem to be solved in the present invention provides the preparation method of the porous carbon cathode material of a kind of safe and reliable, easier industrialization and large-scale production.
For solving the problems of the technologies described above, the inventive method may further comprise the steps:
1), making beating, to be to use water be solvent in making beating, carbon black and binding agent mixed make slurry;
2), dewater, the slurry dehydration that makes;
3), foaming pore-creating, the material after step 2 dehydration is added the thermosetting porous mass,
4), vacuum drying, porous mass is dried.
Above-mentioned steps 1 described making beating also adds when mixing has additive, additive to select the mixture of one or more materials in copper powder, nickel powder, cobalt powder, iron-phthalocyanine, copper phthalocyanine, the cobalt phthalocyanine for use; Described making beating is meant by 5～510: 0～35: 100～3800: 1～58 mass ratio takes by weighing carbon black, additive, water, bonding agent, after earlier bonding agent and water being mixed, add carbon black and additive again, get slurry after usefulness mixer high-speed stirred is even;
Bonding agent in the technique scheme is one or more mixtures in ptfe emulsion, Kynoar emulsion, polyvinyl alcohol water solution, the polyacrylic resin aqueous solution, sodium carboxymethyl cellulose solution, polyacrylamide solution, the cyclodextrin.
Described dewatering process is the combination with one or more methods in filter press dehydration, drier dehydration, the heating, drying dewatering; Described foaming pore-creating technology realizes that by heat the heating, drying temperature is 150～290 ℃, and drying time is 0.1～20h; Described vacuum drying temperature is 100～230 ℃, vacuum degree≤0.1MPa, vacuum drying time 8～25h.
Another technical problem that the present invention will solve provides that a kind of to utilize the carbon cathode material of the porous that above-mentioned preparation method makes be the lithium primary cell that anode makes as the carrier of liquid cathode active material, with the lithium metal.This lithium primary cell production security height, and improve the consistency and the stability of battery electrical property significantly.
Above-mentioned porous carbon cathode material comprises anode and negative electrode as the lithium primary cell of negative electrode, it is characterized in that: described anode is lithium metal or its alloy, and described cathode active material is thionyl chloride SOCl
2, chlorosulfuric acid SO
2Cl
2Or sulfur dioxide SO
2In the liquid cathode active material any one.
The present invention has the following advantages compared to existing technology:
The preparation method of porous carbon cathode material provided by the invention comprises technologies such as making beating, dehydration, foaming, vacuum drying, adopts pure water to replace organic solvents such as isopropyl alcohol of the prior art or alcohol among this preparation method.Pure water is a kind of not volatile, non-flammable liquid, and in operating process, control is not dangerous easily.Because carbon black does not soak in water, the present invention adopts method that high-speed stirred disperses, make carbon black fully disperse in water, evenly mix with material such as binding agent, form the slurry of high dispersive, avoided the reunion and the caking of carbon black, increased the specific area of carbon cathode.So beneficial effect of the present invention is embodied in by high-speed mixing and stirs, solve water effectively and do not soaked into acetylene black, can't be with the uniform problem of mixing of materials of preparation porous carbon cathode material.The strand that the high temperature foaming is actually the binding agent macromolecular material fully stretches, and the distance of carbon black particle is fully drawn back to form spongiform porous material then.So when prior art is used alcohol or isopropyl alcohol and carbon black batch mixing, use mostly and mix mixed, kneading etc. and be similar to " and face " method and carry out batch mixing, carbon black particle can not fully disperse, easily reunion.If adopt prior art only to make water substituted alcohol or isopropyl alcohol mix mixed kneading, because water and carbon black compatibility are poor, not only operation possibility is poor, and the material agglomeration of preparation is more serious.The present invention uses the high speed dispersion machine, stir in airtight container high speed, carbon black is well dispersed in the water, and the strand of high polymer binder is fully stretched, the porous carbon materials pore-size distribution that makes is more even, pore volume is bigger, the specific area of material is bigger, and the liquid cathode active material of storage is more, and catalytic activity is higher, thereby the preparation lithium primary cell in show as discharge voltage higher more steady, discharge capacity is bigger, the consistency of performance is better.Fig. 1 is aperture and the pore volume distribution figure with the carbon cathode of the alcohol mixing procedure of nitrogen absorption BET method mensuration and technology of the present invention making, abscissa is the aperture among the figure, ordinate is a pore volume, the pore-size distribution comparison diagram of the material that makes from two kinds of methods as can be seen, porous carbon materials with the inventive method preparation, pore-size distribution is in narrower range, and pore volume is bigger.With the porous carbon materials that uses alcohol batch mixing and water methods of beating batch mixing to make respectively as cathode current collector, use thionyl chloride to be cathode active material, use lithium metal to be anode, prepare ER14250 type lithium/thinly chloride battery, Fig. 2 is 330 Ω constant-resistance discharge curves under 100 ER14250 type lithium/thinly chloride battery normal temperature making of existing alcohol mixing procedure, Fig. 3 is 330 Ω constant-resistance discharge curves under 100 ER14250 type lithium/thinly chloride battery normal temperature making of technology of the present invention, from Fig. 2 and Fig. 3 more as can be seen, voltage platform in Fig. 3 discharge curve is more stable than Fig. 2's, consistency is better, in addition, be distributed in 80～115h the discharge time among Fig. 2, peak and minimum differ 35h, and be distributed in 88～108h the discharge time among Fig. 3, peak and minimum differ 20h, show that making water is that solvent carries out the porous carbon cathode cell of pulling an oar prepared at a high speed, have high consistency with the discharge performance of the carbon cathode battery of existing technology batch mixing preparation with an organic solvent, discharge voltage plateau is also more steady.
It is decentralized medium that preparation method of the present invention makes water; more safer than organic solvent; the high speed dispersion method of Shi Yonging can adopt existing various high-speed dispersion equipment to realize simultaneously; for example high speed dispersor, duplicate rows star mixer, power mixer, high-shearing dispersion emulsifying machine, homogenizer, power ultrasonic wave dispersing apparatus or the like can directly adopt and realize making beating dispersing technology of the present invention, so easier realization industrialization of the present invention and large-scale production.
Description of drawings:
Fig. 1 is that the alcohol mixing procedure of BET method mensuration and the aperture and the pore volume distribution figure of the carbon cathode that technology of the present invention is made compare;
Fig. 2 is 330 Ω constant-resistance discharge curves under 100 ER14250 type lithium/thinly chloride battery normal temperature making of existing alcohol mixing procedure;
Fig. 3 is 330 Ω constant-resistance discharge curves under 100 ER14250 type lithium/thinly chloride battery normal temperature making of technology of the present invention;
Embodiment
Purport of the present invention is organic solvents such as water substituted alcohol, and water is a kind of not volatile, non-flammable liquid, and in operating process, control is not dangerous easily.Carbon black does not soak in water, the present invention adopt high-speed stirred method, make carbon black in water, fully disperse, evenly mix with compositions such as binding agent and additives, form the water paste of high dispersive, and then obtain the carbon cathode material of porous by dehydration, foaming and vacuum drying prepared.Preparation method of the present invention has solved water effectively and has not soaked into carbon black, can't water as solvent with the problem that carbon black and unclassified stores mix, improved the uniformity and the consistency of electrode.Easier industrialization of negative electrode beating process of the present invention and large-scale production, dehydration and stoving process are safer.And prepare lithium primary cell by this cathode material, the production security height, and improve the consistency and the stability of battery electrical property significantly.
Below in conjunction with embodiment content of the present invention is described in further detail, mentioned content is not a limitation of the invention among the embodiment, and the selection of battery material can be suited measures to local conditions and the result be there is no substantial effect.
Embodiment 1
In order to compare, use existing method to prepare a kind of lithium primary cell porous carbon cathode material, select acetylene black for use, the aqueous emulsion of 60% polytetrafluoroethylene and alcohol, according to acetylene black: polytetrafluoroethylene: the ratio of alcohol quality than 100: 10: 300 adds to mix in the machine of mixing and mixes, extrusion molding is prepared into the carbon bag then, remove alcohol at 90 ℃ of oven dry 10h, high-temperature process foaming 20min under 250～260 ℃ of temperature again, at last at 180 ± 5 ℃, vacuum degree≤-the 0.1MPa condition under vacuum drying 15 ± 2h, obtain the porous carbon cathode material A of finish-drying, as the reference material of existing technology preparation.
Use the inventive method to prepare a kind of lithium primary cell porous carbon cathode material, it be by water making beating, drying dehydration, oven dry further dewater, high temperature foams, vacuum drying technology and making.In its raw material, carbon black is selected acetylene black for use, and binding agent is selected the aqueous emulsion of 60% polytetrafluoroethylene for use.Described water making beating is meant by 5～510: 0～35: 100～3800: 1～58 mass ratio, present embodiment preferably 80: 1500: 8 mass ratio takes by weighing acetylene black, water, ptfe emulsion, after earlier ptfe emulsion and water being mixed, add acetylene black again, with planetary power mixer high-speed stirred, after making each composition fully mix slurry.The slurry of gained put into dewaterer dewater to the moisture mass ratio of slurry be 50～65%, make the carbon bag of suitable shape according to the needs of battery design, under 180 ± 10 ℃ of temperature, dry 5 ± 0.5h then, high temperature foaming 20min under 250～260 ℃ of temperature again, at last 180 ± 5 ℃, vacuum degree≤-the 0.1MPa condition under vacuum drying 15 ± 2h, obtain the porous carbon cathode material B of finish-drying.Use the alcohol imbibition priting to test its porosity up to 90%, aperture and the pore volume distribution situation of using nitrogen absorption BET method to test porous carbon cathode material A and B respectively, see Fig. 1 for details, use the porous carbon cathode material B of the technology of the present invention preparation, the porous carbon cathode material A prepared with prior art compares, pore-size distribution is narrower, and the pore volume in the certain limit is bigger, and this also means to absorb and holds more liquid cathode active material.
Prior art uses batch mixer to mix, and carbon black is kicked up and danced in the air, and environmental pollution is serious, if using a large amount of alcohol or isopropyl alcohol pulls an oar, the one, the inflammable and explosive property of organic solvent makes that the danger of operating process is big, the 2nd, and organic solvent consumption is big, so also be not suitable for the making beating operation.In the technology of the present invention implementation process, be the totally-enclosed container, can not cause kicking up of carbon black in the pulping process and cause workshop condition and pollute because high speed dispersing apparatus such as planetary power mixer uses.Such machine all has pipeline transporter simultaneously; the slurry of the exquisiteness for preparing can be transported in the filter by pipeline and dewater; the cleaning of equipment also is easy to; alleviated labour intensity; basically do not have agglomeration through the carbon black granules that fully disperses under fast state, the porous material that obtains is more even.
Embodiment 2
Prepare a kind of lithium primary cell porous carbon cathode material, it be by the making beating of ultrasonic method water, filter-press dehydration, oven dry further dewater, high temperature foaming, vacuum drying technology and make.In its raw material, carbon black is selected acetylene black for use, and binding agent is selected the aqueous emulsion of 60% polytetrafluoroethylene for use, and functional additive is selected copper powder for use.Present embodiment preferably 300: 20: 3500: 42 mass ratio takes by weighing acetylene black, copper powder, water, ptfe emulsion and mixes, and disperses with power ultrasonic dispersing machine high-speed mixing, after making each composition fully mix slurry.The slurry of gained is by the plate and frame type filter-press filtering means dehydration, after smashing granulation then, oven dry 8h further dewaters under 150 ± 10 ℃ of temperature, high temperature foaming 15min under 280～290 ℃ of temperature again, vacuum drying 17h under 150 ± 5 ℃, vacuum degree≤0.1MPa condition at last obtains the porous carbon cathode material C of finish-drying.
Embodiment 3
Prepare a kind of lithium primary cell porous carbon cathode material, it is to be made by water making beating, drying and dewatering, high temperature foaming, vacuum drying technology.In its raw material, carbon black is selected the mixture of furnace black and conductive carbon black for use, and binding agent is selected the aqueous emulsion of polytetrafluoroethylene and the mixture of the polyacrylic resin aqueous solution for use, and functional additive is selected copper phthalocyanine for use.Present embodiment preferably 100: 3: 3000: 20 mass ratio takes by weighing carbon black, copper phthalocyanine, water and binding agent, wherein carbon black is that mass ratio is 80: 20 the furnace black and the mixture of conductive carbon black, and binding agent is that mass ratio is 60: 40 the aqueous emulsion of polytetrafluoroethylene and the mixture of the polyacrylic resin aqueous solution.After these materials are mixed together, use the high-shearing dispersion emulsifying machine high speed dispersion, after making each composition fully mix fine and smooth slurry.The slurry of gained is by the plate and frame type filter-press filtering means dehydration, after smashing granulation then, under 110 ℃ of temperature, dry 13h, high temperature foaming 50min under 180～200 ℃ of temperature again, vacuum drying 7h under 220 ± 5 ℃, vacuum degree≤0.1MPa condition at last obtains the porous carbon cathode material D of finish-drying.
The porous carbon cathode material is a collector, is again the place of electrochemical reaction, and has certain electro catalytic activity.Prepare the porous carbon cathode particles according to the method described above, storing cathode active material is thionyl chloride SOCl
2Make the porous carbon cathode sheets.And then be prepared into ER14250 type carbon packet mode lithium/thinly chloride battery, carry out constant-resistance discharge with 330 Europe resistance at normal temperatures, note the middle voltage of discharge process and the variation of time, and the voltage-time data of 100 batteries all is depicted as discharge curve in same coordinate.Use discharge curve such as Fig. 2 of the lithium battery of prior art carbon cathode material A preparation, discharge curve such as Fig. 3 of the lithium battery of the technology of the present invention carbon cathode material B preparation.From Fig. 3 and Fig. 2 more as can be seen, the lithium battery of the carbon cathode material of the technology of the present invention gained preparation, its discharge performance has better consistency and voltage stability.For further comparison, use all above-mentioned 4 kinds of carbon cathode material to make the discharge platform voltage (mid-point voltage) of ER14250 type lithium/thinly chloride battery and the distribution situation of discharge time is compared as follows table 1.
Table 1 uses the ER14250 cell discharge performance comparison sheet of various carbon cathode material
| Battery cathode material | Discharge mid-point voltage distribution (V) | Distribute discharge time (h) | Remarks |
| Materials A | ??3.29～3.34 | ??81～112 | Prior art |
| Material B | ??3.28～3.31 | ??88～108 | The technology of the present invention |
| Material C | ??3.33～3.36 | ??89～105 | The technology of the present invention |
| Material D | ??3.38～3.40 | ??83～92 | The technology of the present invention |
From the discharge result of table 1 more as can be seen, use discharge platform voltage ratio prior art more stable of the lithium battery of the technology of the present invention preparation, the consistency of discharge time is better.
Embodiment 4
Equally, prepare 4 kinds of porous carbon cathode sheets according to the method described above respectively, with sulfur dioxide SO
2As cathode active material, use metal lithium sheet as anode, be made into WR34615 type coiling lithium/sulfur dioxide battery, use the 1A current discharge at normal temperatures, resulting discharge curve is compared with the discharge curve of the battery of the carbon cathode material preparation of prior art, has voltage and better discharge consistency more stably.
Embodiment 5
Equally, prepare above-mentioned 4 kinds of carbon cathode sheets according to the method described above respectively, as cathode active material, as anode, be made into half coiling lithium/chlorosulfuric acid battery with metal lithium sheet with chlorosulfuric acid, the stationarity of its discharge and consistency also improve and improve.
Claims (6)
1. the preparation method of a porous carbon cathode material may further comprise the steps:
1), making beating, to be to use water be solvent in making beating, carbon black and binding agent mixed make slurry;
2), dewater, the slurry dehydration that makes;
3), foaming pore-creating, the material after step 2 dehydration is added the thermosetting porous mass;
4), vacuum drying, porous mass is dried.
2. according to the preparation method of the described porous carbon cathode material of claim 1, it is characterized in that: the described making beating of step 1 also adds when mixing has additive, additive to select the mixture of one or more materials in copper powder, nickel powder, cobalt powder, iron-phthalocyanine, copper phthalocyanine, cobalt phthalocyanine, the manganese phthalocyanine for use.
3. according to the preparation method of the described porous carbon cathode material of claim 2, it is characterized in that: described making beating is meant by 5～510: 0～35: 100～3800: 1～58 mass ratio takes by weighing carbon black, additive, water, bonding agent, after earlier bonding agent and water being mixed, add carbon black and additive again, get slurry after usefulness mixer high-speed stirred is even.
4. the preparation method of porous carbon cathode material according to claim 3 is characterized in that: described bonding agent is one or more mixtures in ptfe emulsion, Kynoar emulsion, polyvinyl alcohol water solution, the polyacrylic resin aqueous solution, sodium carboxymethyl cellulose solution, polyacrylamide solution, the cyclodextrin.
5. according to the preparation method of each described a kind of porous carbon cathode material among the claim 1-4, described dewatering process is the combination with one or more methods in filter press dehydration, drier dehydration, the heating, drying method; Described foaming pore-creating technology realizes that by heat the heating, drying temperature is 150～290 ℃, and drying time is 0.1～20h; Described vacuum drying temperature is 100～230 ℃, vacuum degree≤0.1MPa, vacuum drying time 8～25h.
6. a lithium primary cell that uses porous carbon cathode material that the described method of claim 5 makes as negative electrode comprises anode and negative electrode, and it is characterized in that: described anode is lithium metal or its alloy, and described cathode active material is thionyl chloride SOCl
2, chlorosulfuric acid SO
2Cl
2Or sulfur dioxide SO
2In the liquid cathode active material any one.
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| PCT/CN2010/080006 WO2011103760A1 (en) | 2010-02-23 | 2010-12-20 | Preparation method of porous carbon cathode material and primary lithium battery using same material |
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