CN106784734A - A kind of lithium cell cathode material and preparation method thereof - Google Patents
A kind of lithium cell cathode material and preparation method thereof Download PDFInfo
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- CN106784734A CN106784734A CN201710065467.8A CN201710065467A CN106784734A CN 106784734 A CN106784734 A CN 106784734A CN 201710065467 A CN201710065467 A CN 201710065467A CN 106784734 A CN106784734 A CN 106784734A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a kind of lithium cell cathode material and preparation method thereof, the lithium cell cathode material is according to the primary raw material of weight portion：8 10 parts of p-chloromethyl styrene, 2 (N morpholines）10 20 parts of ethane sulfonic acid, 6 (4 aminophenyls) 4,8 15 parts of 5 dihydro 5 methyl 3 (2H) pyridazinone, 28 parts of salicylaldoxime, 13 parts of sodium vinyl sulfonate, 4 (2 ethylamino-) benzene 1,213 parts of diphenol, 2,13 parts of 4 dimethyl pyrrole, 3,5 di-tert-butyl dicarboxylate, 13 parts of nano-structure porous silicon.Organic cathode material of the present invention is using various active mixture as lithium ion battery negative material, the security performance of material and the stability of battery material can be lifted, and the synthetic method of the active material is simple, and technology controlling and process is good, low production cost, energy large-scale application is in industrialized production.
Description
Technical field
The present invention relates to a kind of cell art, specifically a kind of lithium cell cathode material and preparation method thereof.
Background technology
Lithium ion battery negative material main at present mainly has carbons, transition metal oxide, tinbase and silicon substrate etc..
Carbons negative pole has been carried out commercialization at present, but the chemical property of carbons negative pole is poor in low temperature environment, and reason is
Caused by diffusion coefficient of the lithium ion in carbons negative material is low at low ambient temperatures, in addition, the electricity of carbons negative pole removal lithium embedded
Electrode potential is relatively low, and this is easily caused the formation of Li dendrite, and this has had a strong impact on the security performance of lithium ion battery；Oxo transition metal
The greatest problem that compound is used as to exist during lithium ion battery negative material is exactly bad cyclical stability, and capacity attenuation is very fast；And
The problem existed when tinbase and silicon substrate are as lithium ion battery negative material is that such negative material is carrying out meeting when embedding lithium reacts
Up to 300% volumetric expansion is produced, there is larger capacity attenuation and poor capability retention so as to cause such material.
Ion cathode material lithium mentioned above is primarily present the problem in terms of intercalation potential, specific capacity and cyclical stability, it is impossible to very
It is applied in lithium-ion battery system well.Therefore, in order to develop high-energy-density, long circulation life, cheap type lithium ion battery, must
Must exploitation novel cathode material for lithium ion battery.
The content of the invention
It is an object of the invention to provide a kind of lithium cell cathode material and preparation method thereof, to solve above-mentioned background technology
The problem of middle proposition.
To achieve the above object, the present invention provides following technical scheme：
A kind of lithium cell cathode material, be according to the primary raw material of weight portion：P-chloromethyl styrene 8-10 parts, 2- (N- morpholines）
Ethane sulfonic acid 10-20 parts, 8-15 parts of -3 (2H)-pyridazinone of 6- (4- aminophenyls) -4,5- dihydro -5- methyl, salicylaldoxime 2-8
Part, sodium vinyl sulfonate 1-3 parts, 1-3 parts of 4- (2- ethylamino-s) benzene -1,2- diphenol, 2,4- dimethyl pyrrole -3,5- dicarboxylic acids two
Tert-butyl ester 1-3 parts, nano-structure porous silicon 1-3 parts.
As further scheme of the invention：The lithium cell cathode material, be according to the primary raw material of weight portion：To chlorine
Methyl styrene 8-10 parts, 2- (N- morpholines）Ethane sulfonic acid 12-18 parts, 6- (4- aminophenyls) -4,5- dihydro -5- methyl -3
11-13 parts of (2H)-pyridazinone, salicylaldoxime 3-7 parts, sodium vinyl sulfonate 1-3 parts, 4- (2- ethylamino-s) benzene -1,2- diphenol 1-3
Part, 1-3 parts, nano-structure porous silicon 1-3 parts of 2,4- dimethyl pyrroles -3,5- di-tert-butyl dicarboxylates.
As further scheme of the invention：The lithium cell cathode material, be according to the primary raw material of weight portion：To chlorine
9 parts of methyl styrene, 2- (N- morpholines）15 parts of ethane sulfonic acid, 6- (4- aminophenyls) -4,5- dihydro -5- methyl -3 (2H)-rattle away
12 parts of piperazine ketone, 5 parts of salicylaldoxime, 2 parts of sodium vinyl sulfonate, 2 parts of 4- (2- ethylamino-s) benzene -1,2- diphenol, 2,4- dimethyl pyrazoles
Cough up 2 parts of -3,5- di-tert-butyl dicarboxylates, 2 parts of nano-structure porous silicon.
A kind of preparation method of lithium cell cathode material, concretely comprises the following steps：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 2-4h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene-
1,2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 5-8MPa, are controlled
Temperature processed is 42-50 DEG C, is obtained final product.
As further scheme of the invention：Step（1）In be then forced into 7MPa, control temperature be 46 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：
Organic cathode material of the present invention, as lithium ion battery negative material, can lift material using various active mixture
The stability of security performance and battery material, and the synthetic method of the active material is simple, and technology controlling and process is good, is produced into
This is low, and energy large-scale application is in industrialized production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of lithium cell cathode material, be according to the primary raw material of weight portion：8 parts of p-chloromethyl styrene, 2- (N- morpholines）Second
10 parts of alkyl sulfonic acid, 8 parts of -3 (2H)-pyridazinone of 6- (4- aminophenyls) -4,5- dihydro -5- methyl, 2 parts of salicylaldoxime, vinyl
1 part of sodium sulfonate, 1 part of 4- (2- ethylamino-s) benzene -1,2- diphenol, 1 part of 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, receive
1 part of porous silicon of rice.
A kind of preparation method of lithium cell cathode material, concretely comprises the following steps：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 2h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene -1,
2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 5MPa, control temperature
It is 42 DEG C to spend, and is obtained final product.
Embodiment 2
A kind of lithium cell cathode material, be according to the primary raw material of weight portion：8 parts of p-chloromethyl styrene, 2- (N- morpholines）Second
12 parts of alkyl sulfonic acid, 11 parts of -3 (2H)-pyridazinone of 6- (4- aminophenyls) -4,5- dihydro -5- methyl, 3 parts of salicylaldoxime, vinyl
1 part of sodium sulfonate, 1 part of 4- (2- ethylamino-s) benzene -1,2- diphenol, 1 part of 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, receive
1 part of porous silicon of rice.
A kind of preparation method of lithium cell cathode material, concretely comprises the following steps：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 2h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene -1,
2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 5MPa, control temperature
It is 44 DEG C to spend, and is obtained final product.
Embodiment 3
A kind of lithium cell cathode material, be according to the primary raw material of weight portion：9 parts of p-chloromethyl styrene, 2- (N- morpholines）Second
15 parts of alkyl sulfonic acid, 12 parts of -3 (2H)-pyridazinone of 6- (4- aminophenyls) -4,5- dihydro -5- methyl, 5 parts of salicylaldoxime, vinyl
2 parts of sodium sulfonate, 2 parts of 4- (2- ethylamino-s) benzene -1,2- diphenol, 2 parts of 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, receive
2 parts of porous silicon of rice.
A kind of preparation method of lithium cell cathode material, concretely comprises the following steps：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 3h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene -1,
2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 7MPa, control temperature
It is 46 DEG C to spend, and is obtained final product.
Embodiment 4
A kind of lithium cell cathode material, be according to the primary raw material of weight portion：10 parts of p-chloromethyl styrene, 2- (N- morpholines）Second
18 parts of alkyl sulfonic acid, 13 parts of -3 (2H)-pyridazinone of 6- (4- aminophenyls) -4,5- dihydro -5- methyl, 7 parts of salicylaldoxime, vinyl
3 parts of sodium sulfonate, 3 parts of 4- (2- ethylamino-s) benzene -1,2- diphenol, 3 parts of 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, receive
3 parts of porous silicon of rice.
A kind of preparation method of lithium cell cathode material, concretely comprises the following steps：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 4h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene -1,
2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 7MPa, control temperature
It is 48 DEG C to spend, and is obtained final product.
Embodiment 5
A kind of lithium cell cathode material, be according to the primary raw material of weight portion：10 parts of p-chloromethyl styrene, 2- (N- morpholines）Second
20 parts of alkyl sulfonic acid, 15 parts of -3 (2H)-pyridazinone of 6- (4- aminophenyls) -4,5- dihydro -5- methyl, 8 parts of salicylaldoxime, vinyl
3 parts of sodium sulfonate, 3 parts of 4- (2- ethylamino-s) benzene -1,2- diphenol, 3 parts of 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, receive
3 parts of porous silicon of rice.
A kind of preparation method of lithium cell cathode material, concretely comprises the following steps：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 4h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene -1,
2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 8MPa, control temperature
It is 50 DEG C to spend, and is obtained final product.
Test experiments：
Organic cathode material prepared by embodiment 1-5 is prepared into 1665132 model lithium-ion-power cells（Model H16*W65*
The lamination soft-package battery of L132mm）, compacted density is in 3.0g/cm3More than, volume energy density is in more than 450Wh/L；Battery core exists
Under 3.0V-4.2V voltages, 1C electric discharge gram volumes play more than 120mAh/g；1C charge and discharges circulate 2000 capacity and are maintained under normal temperature
More than 94%；Electric discharge is more than the 98% of 1C capacity under 6C multiplying powers；3C/10V overcharges test, and battery is not on fire does not explode；High temperature circulation
Excellent, 1C charge and discharges circulate 1000 capacity and are maintained at more than 92% at 60 DEG C；With good security performance, acupuncture, extruding, mistake
Fill, cross put etc. test do not explode, it is not on fire；And first week specific discharge capacity is 852.6-958.9mAh/g, charging quality specific capacity
It is 534.9-568.8mAh/g, charging quality specific capacity is maintained at 498.6-543.4mAh/g, specific discharge capacity after circulation in 40 weeks
It is 532.7-561.3Ah/g, with good cycle performance.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires to be limited rather than described above, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.
Claims (5)
1. a kind of lithium cell cathode material, it is characterised in that the primary raw material according to weight portion is：P-chloromethyl styrene 8-10
Part, 2- (N- morpholines）Ethane sulfonic acid 10-20 parts, (the 2H)-pyridazinone 8-15 of 6- (4- aminophenyls) -4,5- dihydro -5- methyl -3
Part, salicylaldoxime 2-8 parts, sodium vinyl sulfonate 1-3 parts, 1-3 parts of 4- (2- ethylamino-s) benzene -1,2- diphenol, 2,4- dimethyl pyrazoles
Cough up 1-3 parts, nano-structure porous silicon 1-3 parts of -3,5- di-tert-butyl dicarboxylates.
2. lithium cell cathode material according to claim 1, it is characterised in that the lithium cell cathode material, according to weight
Measure part primary raw material be：P-chloromethyl styrene 8-10 parts, 2- (N- morpholines）Ethane sulfonic acid 12-18 parts, 6- (4- aminobenzenes
Base) 11-13 parts of -3 (2H)-pyridazinone of -4,5- dihydro -5- methyl, salicylaldoxime 3-7 parts, sodium vinyl sulfonate 1-3 parts, 4- (2-
Ethylamino-) 1-3 parts of benzene -1,2- diphenol, 1-3 parts of 2,4- dimethyl pyrroles -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon 1-3
Part.
3. lithium cell cathode material according to claim 1 and 2, it is characterised in that the lithium cell cathode material, according to
The primary raw material of weight portion is：9 parts of p-chloromethyl styrene, 2- (N- morpholines）15 parts of ethane sulfonic acid, 6- (4- aminophenyls) -4,
12 parts of -3 (2H)-pyridazinone of 5- dihydro -5- methyl, 5 parts of salicylaldoxime, 2 parts of sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene -1,
2 parts of 2- diphenol, 2 parts of 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, 2 parts of nano-structure porous silicon.
4. a kind of preparation method of lithium cell cathode material as described in claim 1-3 is any, it is characterised in that specific steps
For：
First, p-chloromethyl styrene, 6- (4- aminophenyls)-(2H)-pyridazinone of 4,5- dihydro -5- methyl -3 are total to
Mixed, ice bath 2-4h is subsequently added 2- (N- morpholines）Ethane sulfonic acid, salicylaldoxime, sodium vinyl sulfonate, 4- (2- ethylamino-s) benzene-
1,2- diphenol, 2,4- dimethyl pyrrole -3,5- di-tert-butyl dicarboxylates, nano-structure porous silicon are mixed, and are then forced into 5-8MPa, are controlled
Temperature processed is 42-50 DEG C, is obtained final product.
5. the preparation method of lithium cell cathode material according to claim 4, it is characterised in that step（1）In then plus
7MPa is depressed into, it is 46 DEG C to control temperature.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101510602A (en) * | 2009-02-19 | 2009-08-19 | 上海交通大学 | Method for preparing silicon composite cathode material of lithium ion battery |
| CN104966839A (en) * | 2015-07-15 | 2015-10-07 | 山东大学 | Lithium battery negative electrode material modifying method |
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2017
- 2017-02-06 CN CN201710065467.8A patent/CN106784734A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101510602A (en) * | 2009-02-19 | 2009-08-19 | 上海交通大学 | Method for preparing silicon composite cathode material of lithium ion battery |
| CN104966839A (en) * | 2015-07-15 | 2015-10-07 | 山东大学 | Lithium battery negative electrode material modifying method |
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Application publication date: 20170531 |