CN105932294A - Nanocarbon conductive paste used for lead-acid storage battery, preparation method and application for nanocarbon conductive paste - Google Patents
Nanocarbon conductive paste used for lead-acid storage battery, preparation method and application for nanocarbon conductive paste Download PDFInfo
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- CN105932294A CN105932294A CN201610546870.8A CN201610546870A CN105932294A CN 105932294 A CN105932294 A CN 105932294A CN 201610546870 A CN201610546870 A CN 201610546870A CN 105932294 A CN105932294 A CN 105932294A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/14—Electrodes for lead-acid accumulators
- H01M4/16—Processes of manufacture
-
- 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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/14—Electrodes for lead-acid accumulators
- H01M4/16—Processes of manufacture
- H01M4/20—Processes of manufacture of pasted electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of the lead-acid storage battery. The invention discloses nanocarbon conductive paste used for the lead-acid storage battery and a preparation method for the nanocarbon conductive paste. The preparation method comprises the following steps of mixing a nanocarbon material with a sulfuric acid oxidized liquid, then carrying out heating and refluxing, keeping the slight boiling state of the paste by ultrasonic at the same time; and obtaining the fully oxidized nanocarbon conductive paste after a certain time reaction. The prepared conductive paste is used to replace sulfuric acid to prepare a battery polar plate; and the charging receptivity, the low-temperature performance, the HRPSoC and the SBA cycling service life of the lead-acid storage battery adopting the polar plate are obviously improved.
Description
Technical field
The invention belongs to Lead-acid Battery Technology field, be specifically related to the preparation method of nano-sized carbon electrocondution slurry
And the application in lead-acid battery.
Background technology
Lead-acid battery is abundant with its raw material sources, cost performance high, security reliability is good, recoverable
Etc. advantage, occupy critical role in secondary power supply field.In electric or hybrid automobile and intermittence
In the application such as energy-storage system, it is desirable to lead-acid battery has more excellent charge acceptance and cycle life.
And traditional lead acid batteries is under above-mentioned operating mode, negative terminal surface easily forms thick lead sulfate crystal, these
Crystal is in charging process subsequently, it is impossible to be fully converted to metallic lead, thus can reduce charge efficiency and
Cycle life.
In lead-acid battery cathode lead plaster, add material with carbon element, its charge acceptance can be improved, suppress table
The irreversible sulfation in face, makes battery have high power capacity and high-power characteristic concurrently.Carbon is added in positive pole,
Its active material utilization, threadiness or lamellar material with carbon element can be provided, active substance can be improved simultaneously
Structural strength.
Owing to carbon is different with the proportion of lead, most of material with carbon elements are difficult to be directly added into lead plaster and reach the most mixed
Close.Therefore, how nano-sized carbon being dispersed in simply, efficiently in lead carbon battery lead plaster is to be badly in need of at present solving
Problem certainly.
Summary of the invention
The present invention solves above-mentioned technical problem, it is provided that a kind of nano-sized carbon for lead-acid accumulator is conducted electricity
Slurry, preparation method and application, provide for dispersed in lead-acid battery electrode plate of nano-carbon material
A kind of preparation method simple, efficient.
The technical scheme that a first aspect of the present invention provides is: a kind of nano-sized carbon for lead-acid accumulator is led
The preparation method of plasma-based material, it is characterised in that comprise the steps: nano-carbon material and sulfuric acid oxidation
Liquid mixes, and is then heated to reflux, simultaneously with ultrasonic holding slurry slight boiling condition, after reaction certain time,
Obtain fully oxidized nano-sized carbon electrocondution slurry.
Preferably, in described nano-sized carbon electrocondution slurry, the content of nano-sized carbon is 1～20wt.%.
Preferably, in described sulfuric acid oxidation liquid, oxide isolation include but not limited to sulphuric acid, hydrogen peroxide,
Ozone, nitric acid, ammonium nitrate.Preferred sulfuric acid concentration is 50～100%.
Preferably, one during described nano-carbon material is CNT, Graphene, Nano graphite powder or
Several.
Preferably, described nano-sized carbon reflux time in sulphuric acid is 0.5～5 hour, reflux temperature
It it is 80～250 DEG C.
In currently preferred technical scheme, the ultrasonic power that described ultrasonic disperse uses is 10～100
W/L；And during being heated to reflux, preferably it is passed through ozone.
In currently preferred technical scheme, the preparation method of a kind of nano-sized carbon electrocondution slurry, including such as
Lower step: take sulfuric acid oxidation liquid, adds nano-carbon material under stirring, then passes to ozone and carry out
It is heated to reflux, simultaneously with ultrasonic holding slurry slight boiling condition, reacts 0.5-3 hour, after cooling, i.e.
Obtain nano-sized carbon electrocondution slurry.
A second aspect of the present invention provides a kind of nano-sized carbon electrocondution slurry for lead-acid accumulator, and it is by such as
Lower section method prepares: is mixed with sulfuric acid oxidation liquid by nano-carbon material, is then heated to reflux, accompanies simultaneously
With ultrasonic holding slurry slight boiling condition, after reaction certain time, obtain fully oxidized nano-sized carbon conductive paste
Material.
A third aspect of the present invention provides the purposes of the nano-sized carbon electrocondution slurry for lead-acid accumulator, nanometer
Carbonaceous conductive slurry substitutes liquid as sulphuric acid, for the preparation of lead-acid battery positive and negative electrode lead plaster, through coated plate,
Solidification, dry positive and negative electrode pole plate of making, more i.e. obtain lead-acid battery after assembling, chemical conversion.
Preferably, in the equally distributed lead plaster of described nano-sized carbon, nano-sized carbon content is 0.05～5wt.%.
The preparation method of lead-acid battery cathode pole plate is: be poured slowly into continuously stirred by nano-sized carbon electrocondution slurry
Equal-volume water in, diluted for use；Take Hydrocerussitum (Ceruse), extender, after chopped fiber mix homogeneously, quickly add water
Stirring mixing, is slowly added to the sulphuric acid of certain density, then proceedes to be slowly added to nano-sized carbon electrocondution slurry,
Mix homogeneously after all adding, through coated plate, solidification, dried, i.e. obtains CNT equally distributed
Negative plates.
The preparation method of lead-acid battery anode plate: nano-sized carbon electrocondution slurry is poured slowly into continuously stirred
In equal-volume water, diluted for use；Taking Hydrocerussitum (Ceruse), after chopped fiber mix homogeneously, quickly add water stirring mixing,
It is slowly added to the sulphuric acid of certain density, then proceedes to be slowly added to nano-sized carbon electrocondution slurry, after all adding
Mixing, through coated plate, solidification, dried, i.e. obtains the anode plate of the uniform cloth of CNT.
It is an advantage of the current invention that: the invention provides the preparation method of a kind of lead-acid battery electrode plate, nanometer
Material with carbon element being uniformly dispersed in electrocondution slurry, is improve the performance of battery pole plates, and is effectively shortening life
Product cycle and control cost, promote the promotion and application of high-performance lead-acid battery.The present invention prepares
Electrocondution slurry replacement sulfur processed with acid makees battery pole plates.Use the lead-acid battery of this pole plate, its charge acceptance,
Cryogenic property, HRPSoC and SBA cycle life are improved significantly.
Accompanying drawing explanation
The SEM photograph of Fig. 1 crystal whisker-shaped carbon nanotube.
The infared spectrum of Fig. 2 oxide/carbon nanometer tube.
The SEM photograph of the lead-acid battery cathode material that Fig. 3 the inventive method prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiments are
For illustrating that the present invention is not limited to limit the scope of the present invention.The implementation condition used in embodiment is permissible
Condition according to concrete producer does adjustment further, and not marked implementation condition is usually in normal experiment
Condition.
Reference examples 1
Anode plate: employing 230kg Hydrocerussitum (Ceruse), 150g chopped fiber, after mixing homogeneously with 30L water slowly
Adding 25.9kg density is the sulfuric acid solution of 1.4g/ml, uniformly makes anode diachylon after mixing.Through coated plate,
Solidification, dried, i.e. obtain anode plate.
Negative plates: use 230kg Hydrocerussitum (Ceruse), 150g chopped fiber, 1.4kg extender, mix with 27L water
It is slowly added to, after closing uniformly, the sulfuric acid solution that 23.1kg density is 1.4g/ml, uniformly makes negative pole after mixing
Lead plaster.Through coated plate, solidification, dried, i.e. obtain negative plates.
Embodiment 1
Anode plate: employing 230kg Hydrocerussitum (Ceruse), 150g chopped fiber, after mixing homogeneously with 30L water slowly
Adding 25.9kg density is the sulfuric acid solution of 1.4g/ml, uniformly makes lead plaster after mixing.Through coated plate, admittedly
Change, dried, i.e. obtain anode plate.
Negative plates: take 7.5L concentrated sulfuric acid solution (97%), then proceedes to stirring and in mixed liquor
Add 375g Suzhou the first element Nanosolutions GmbH crystal whisker-shaped carbon nanotube (long 5-10um,
Diameter 50～90nm, purity is more than 97%, such as Fig. 1).At the beginning for the treatment of that CNT complete wetting i.e. obtains
Beginning slurry.Above-mentioned slurry is heated to reflux temperature, and makes slurry keep slight boiling condition, instead with ultrasonic
1 hour should be continued, then natural cooling, i.e. obtain pre-dispersed CNT/sulphuric acid slurry.By upper
Stating slurry to be poured slowly in continuously stirred 7.5L water, be diluted to 15L slurry standby, wherein sulphuric acid is molten
Liquid-tight degree is 1.4g/ml.Take Hydrocerussitum (Ceruse) (oxidizability 70%) 230kg, extender 1.4kg, chopped fiber
After the mix homogeneously such as 150g, the 19.5L that quickly adds water stirring mixing 15min, it is slowly added to density 1.4g/ml
Sulphuric acid 1.5L, then proceed to be slowly added to CNT/sulphuric acid slurry 15L altogether, mixed after all adding
Close uniformly, through coated plate, solidification, dried, i.e. obtain the equally distributed negative plates of CNT.
Embodiment 2
Anode plate: take 7.5L concentrated sulfuric acid solution (97%), continues stirring and adds in mixed liquor
Crystal whisker-shaped carbon nanotube (long 5-10um, the diameter of 500g Suzhou the first element Nanosolutions GmbH
50～90nm, purity is more than 97%, such as Fig. 1).Treat that CNT complete wetting i.e. obtains initial slurry.
In above-mentioned slurry, it is continually fed into ozone, is heated to reflux temperature, and with ultrasonic holding slurry micro-boiling shape
State, reaction continues 2 hours, then after natural cooling, stops ozone, i.e. obtains pre-dispersed carbon nanometer
Pipe/sulphuric acid slurry.Above-mentioned slurry is poured slowly in continuously stirred 7.5L water, is diluted to 15L slurry
Expecting standby, wherein sulfuric acid solution density is 1.4g/ml.Take Hydrocerussitum (Ceruse) (oxidizability 70%) 230kg, short
After the mix homogeneously such as fiber 150g, the 22.5L that quickly adds water stirring mixing 15min, it is slowly added to density
The sulphuric acid 3.5L of 1.4g/ml, then proceedes to be slowly added to CNT/sulphuric acid slurry 15L altogether, all
After mixing 15min after addition, i.e. obtain anode diachylon.Through coated plate, solidification, dried, i.e. obtain
The anode plate of the uniform cloth of CNT.
Negative plates: take 7.5L concentrated sulfuric acid solution (97%), then proceedes to stirring and in mixed liquor
Add 375g Suzhou the first element Nanosolutions GmbH crystal whisker-shaped carbon nanotube (long 5-10um,
Diameter 50～90nm, purity is more than 97%, such as Fig. 1).At the beginning for the treatment of that CNT complete wetting i.e. obtains
Beginning slurry.Above-mentioned slurry is heated to reflux temperature, and makes slurry keep slight boiling condition, instead with ultrasonic
1 hour should be continued, then natural cooling, i.e. obtain pre-dispersed CNT/sulphuric acid slurry.By upper
Stating slurry to be poured slowly in continuously stirred 7.5L water, be diluted to 15L slurry standby, wherein sulphuric acid is molten
Liquid-tight degree is 1.4g/ml.Take Hydrocerussitum (Ceruse) (oxidizability 70%) 230kg, extender 1.4kg, chopped fiber
After the mix homogeneously such as 150g, the 19.5L that quickly adds water stirring mixing 15min, it is slowly added to density 1.4g/ml
Sulphuric acid 1.5L, then proceed to be slowly added to CNT/sulphuric acid slurry 15L altogether, mixed after all adding
Close uniformly, through coated plate, solidification, dried, i.e. obtain the equally distributed negative plates of CNT.
The reference cell that battery is common processes and prepared by formula of above reference examples 1 preparation, embodiment 1
CNT is with the addition of with the form of sulphuric acid slurry, positive and negative in embodiment 2 in negative electrode active material
Pole active substance all with the addition of CNT with the form of sulphuric acid slurry.It is wherein sulfuric acid treatment such as Fig. 2
The infared spectrum of the CNT crossed, it can be seen that carbon nano tube surface has been grafted carboxyl and hydroxyl.By lead
Acid battery is common and cream technique mixes, and i.e. can get the equally distributed lead plaster of CNT, such as figure
3。
The pole plate respectively prepared by reference examples 1, embodiment 1, embodiment 2 assembled by same process and
Chemical conversion, obtains testing battery.By the following method, the battery that prepared by test above-described embodiment.
Individually below negative pole is added nano-sized carbon and positive and negative electrode all adds lead carbon battery and the reference of nano-sized carbon
Battery contrasts, its test result such as following table.
The test result contrasting above battery compartment key performance understands, the lead carbon battery that this patent provides
Preparation method, not only substantially reduces cycle and cost that nano-sized carbon is applied from pretreatment to reality, and
Nano-carbon material being uniformly distributed in lead plaster, reduces the gassing rate being filled with every ampere-hour electricity, hence it is evident that carry
Circulation under high charge acceptance, low temperature capacity, the cycle life of partial state of charge state and start-stop operating mode
Life-span, the combination property of significant increase battery and cost performance.
Examples detailed above only for technology design and the feature of the present invention are described, its object is to allow and is familiar with this skill
The people of art is to will appreciate that present disclosure and implement according to this, can not limit the protection of the present invention with this
Scope.All equivalent transformations done according to spirit of the invention or modification, all should contain the present invention's
Within protection domain.
Claims (10)
1. the preparation method for the nano-sized carbon electrocondution slurry of lead-acid accumulator, it is characterized in that, comprise the steps: to mix nano-carbon material with sulfuric acid oxidation liquid, then it is heated to reflux, simultaneously with ultrasonic holding slurry slight boiling condition, after reaction certain time, obtain fully oxidized nano-sized carbon electrocondution slurry.
Preparation method the most according to claim 1, it is characterised in that in described nano-sized carbon electrocondution slurry, the content of nano-sized carbon is 1～20wt.%.
Preparation method the most according to claim 1, it is characterised in that the oxide isolation of described sulfuric acid oxidation liquid is selected from sulphuric acid, hydrogen peroxide, ozone, nitric acid, ammonium nitrate.
Preparation method the most according to claim 1, it is characterised in that described nano-carbon material is one or more in CNT, Graphene, Nano graphite powder.
Preparation method the most according to claim 1, it is characterised in that described nano-sized carbon reflux time in sulphuric acid is 0.5～5 hour, reflux temperature is 80～250 DEG C.
6. the nano-sized carbon electrocondution slurry for lead-acid accumulator, it prepares by the following method: is mixed with sulfuric acid oxidation liquid by nano-carbon material, is then heated to reflux, simultaneously with ultrasonic holding slurry slight boiling condition, after reaction certain time, obtain fully oxidized nano-sized carbon electrocondution slurry.
7. the purposes of the nano-sized carbon electrocondution slurry for lead-acid accumulator as claimed in claim 6, it is characterized in that, nano-sized carbon electrocondution slurry substitutes liquid as sulphuric acid, preparation for lead-acid battery positive and negative electrode lead plaster, through coated plate, solidify, be dried and make positive and negative electrode pole plate, more i.e. obtain lead-acid battery after assembling, chemical conversion.
Purposes the most according to claim 7, it is characterised in that in the equally distributed lead plaster of described nano-sized carbon, nano-sized carbon content is 0.05～5wt.%.
Purposes the most according to claim 7, it is characterised in that the preparation method of lead-acid battery cathode pole plate is: nano-sized carbon electrocondution slurry is poured slowly in continuously stirred equal-volume water, diluted for use；Taking Hydrocerussitum (Ceruse), extender, after chopped fiber mix homogeneously, quickly add water stirring mixing, is slowly added to the sulphuric acid of certain density, then proceedes to be slowly added to nano-sized carbon electrocondution slurry, mix homogeneously after all adding, through coated plate, solidification, dried, i.e. obtains the equally distributed negative plates of CNT.
Purposes the most according to claim 7, it is characterised in that the preparation method of lead-acid battery anode plate: nano-sized carbon electrocondution slurry is poured slowly in continuously stirred equal-volume water, diluted for use；Taking Hydrocerussitum (Ceruse), after chopped fiber mix homogeneously, quickly add water stirring mixing, it is slowly added to the sulphuric acid of certain density, then proceedes to be slowly added to nano-sized carbon electrocondution slurry, mix homogeneously after all adding, through coated plate, solidification, dried, i.e. obtain the anode plate of the uniform cloth of CNT.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113161539A (en) * | 2021-02-05 | 2021-07-23 | 肇庆理士电源技术有限公司 | Trace acidized carbon nanotube negative plate and lead paste and preparation method thereof |
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| CN102064319A (en) * | 2010-12-14 | 2011-05-18 | 哈尔滨工业大学 | Negative plate of lead acid super battery, production method and lead acid super battery assembled by negative plate |
| CN102646821A (en) * | 2012-05-08 | 2012-08-22 | 电子科技大学 | Preparing method of negative materials for lithium ion batteries |
| WO2014030169A1 (en) * | 2012-08-23 | 2014-02-27 | Director General, Defence Research & Development Organisation | Process for synthesizing hybride bifunctionalized multiwalled carbon nanotubes and applications thereof |
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2016
- 2016-07-13 CN CN201610546870.8A patent/CN105932294A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102064319A (en) * | 2010-12-14 | 2011-05-18 | 哈尔滨工业大学 | Negative plate of lead acid super battery, production method and lead acid super battery assembled by negative plate |
| CN102646821A (en) * | 2012-05-08 | 2012-08-22 | 电子科技大学 | Preparing method of negative materials for lithium ion batteries |
| WO2014030169A1 (en) * | 2012-08-23 | 2014-02-27 | Director General, Defence Research & Development Organisation | Process for synthesizing hybride bifunctionalized multiwalled carbon nanotubes and applications thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113161539A (en) * | 2021-02-05 | 2021-07-23 | 肇庆理士电源技术有限公司 | Trace acidized carbon nanotube negative plate and lead paste and preparation method thereof |
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Application publication date: 20160907 |