CN109860531A - A kind of nanometer of lead/carbon composite preparation method and application - Google Patents
A kind of nanometer of lead/carbon composite preparation method and application Download PDFInfo
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- CN109860531A CN109860531A CN201811538256.2A CN201811538256A CN109860531A CN 109860531 A CN109860531 A CN 109860531A CN 201811538256 A CN201811538256 A CN 201811538256A CN 109860531 A CN109860531 A CN 109860531A
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Abstract
The invention discloses a kind of nanometer of lead/carbon composite preparation method and application.The preparation method carries out in accordance with the following steps: (1) carbon material being added in aqueous oxidizing agent solution and carry out oxidation processes, obtain mixed liquor A；(2) aqueous solution in lead source is mixed with mixed liquor A, stirring 0.5 hour or more, so that lead ion is adsorbed on the surface of carbon material, obtain mixed liquid B；(3) surfactant is added into mixed liquid B, stirring 0.5 hour or more, then filtered, be dried in vacuo to obtain presoma；(4) in protective atmosphere, 300-700 DEG C of roasting is carried out to gained presoma, a nanometer lead/carbon composite is obtained after heat treatment.Application the present invention provides nanometer lead/carbon composite as super lead carbon battery negative electrode active material.The preparation method of nanometer lead/carbon composite of the present invention is easy to operate, and obtained lead particle size is minimum and is evenly dispersed on the surface of carbon material, which can preferably inhibit evolving hydrogen reaction.
Description
Technical field
The present invention relates to a kind of nanometer of lead/carbon composite preparation method and the applications in super lead carbon battery.
Background technique
Lead-acid battery is cheap with its, using the advantages such as safe, use temperature range is wide in middle low-speed electronic vehicle field
Occupy staple market.But traditional lead-acid accumulator service life is not grown, cycle life differs in 300-500 weeks, still
The super lead carbon battery cycle life that introducing carbon material is opened up in cathode can be improved 3-6 times and differ.Super lead carbon battery is
A kind of novel battery of the capacitance characteristic combining carbon material and lead-acid battery high-energy-density advantage tests verified super lead
Carbon battery has very big advantage in terms of (- 18 DEG C) of low temperature electric discharges and heavy-current discharge.
Super lead carbon battery solves that cycle life of the traditional lead acid batteries under high magnification partial state of charge is short to ask
Topic, but actual market is very high to the expectation of super lead carbon battery, it is not able to satisfy the market demand at present.It chases after and traces it to its cause
In: in cyclic process, the carbon in cathode is easy electrolysis water and hydrogen is precipitated super lead carbon battery.Since the hydrogen of generation is excessive,
The oxygen that can not be generated in time with anode reacts to form water, is largely precipitated from inside battery, eventually leads to water in electrolyte and contain
Amount is reduced, and sour specific gravity increases, and leads to battery end of life.
In order to solve this problem, it has been proposed that the metallic lead of high overpotential of hydrogen evolution is loaded on carbon to inhibit liberation of hydrogen anti-
It answers.The method of load is usually to mix the biomass such as lead salt and starch, maize flour in water, then passes through the behaviour such as roasting again
Make, finally obtains lead carbon composite.This process is sufficiently complex, and carbon source is biomass, the carbon material formed after being fired
Middle impurity content is more, and part of impurity (chlorine, iron etc.) can increase the self-discharge rate of battery, institute in super lead carbon battery
It is very low to require its content.
Therefore, it is necessary to develop a kind of preparation method of lead carbon composite simpler in operation, and make lead/carbon
Composite material can preferably inhibit evolving hydrogen reaction, and then improve the cycle life of super lead carbon battery.
Summary of the invention
It is born the object of the present invention is to provide a kind of nanometer of lead/carbon composite preparation method and as super lead carbon battery
The application of pole active material.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of nanometer of lead/carbon composite preparation method carries out in accordance with the following steps:
(1) carbon material is added in aqueous oxidizing agent solution and carries out oxidation processes, to improve the oxygen-containing function of carbon material surface
Group's quantity, obtains mixed liquor A；
(2) aqueous solution in lead source is mixed with mixed liquor A, stirring 0.5 hour or more (preferably 0.5-1 hours), make lead from
Son is adsorbed on the surface of carbon material, obtains mixed liquid B；
(3) surfactant is added into mixed liquid B, stirring 0.5 hour or more (preferably 0.5-1 hours), then passes through
Filter, vacuum drying obtain presoma；
(4) in protective atmosphere, 300-700 DEG C of roasting is carried out to gained presoma, final product is obtained after heat treatment and receives
Rice lead/carbon composite.
The preparation method of nanometer lead/carbon composite of the present invention, core are first to aoxidize carbon material,
The purpose of oxidation is the oxygen-containing functional group quantity of raising carbon material surface, and oxygen-containing functional group not only facilitates the suction of lead ion
It is attached, it is better able to improve the overpotential of hydrogen evolution of carbon material itself；Then strong suction of the oxygen-containing functional group to heavy metal lead ion is utilized
Attached property, makes lead ion equably be adsorbed on the surface of carbon material, roasts finally by protection gas, due to carbon (and hydrogen)
Reproducibility finally obtains a nanometer lead/carbon composite.In the nanometer lead/carbon composite, the granular size of nanometer lead is
50nm is hereinafter, nanometer lead particle is evenly dispersed on the surface of carbon material.
Preferably, the carbon material is the carbon material with high hydrogen-evolution overpotential and high capacitance characteristic, high hydrogen-evolution overpotential
Carbon material can reduce the fluid loss of battery, the carbon material of high capacitance can make battery play buffering in high current charge-discharge
Effect, wherein at least 1.0V or more (reference electrode is mercury/Mercurous sulfate electrode), specific capacitance at least exists overpotential of hydrogen evolution
(electrolyte of test is the sulfuric acid solution of 1.28g/ml to 150F/g or more, is platinum electrode to electrode, reference electrode is mercury/sulfuric acid
Mercurous electrode).As a further preference, the carbon material is selected from least one of rice hull carbon, graphene, coconut carbon.
Preferably, the oxidant is hydrogen peroxide and/or nitric acid.
Preferably, the concentration of oxidant is 3-30% in aqueous oxidizing agent solution；The volume of the aqueous oxidizing agent solution is used
Amount is calculated as 20-1600mL/g, more preferably 20-300mL/g with the quality of carbon material.
Preferably, the lead source is selected from least one of plumbi nitras, lead acetate, lead chloride.
Preferably, the mass concentration of the aqueous solution in the lead source is 1.5-10%, more preferably 1.96-9.09%.
Preferably, the feed ratio of the lead source and carbon material is calculated as 0.5-40 with the mass ratio of lead and carbon material, it is more excellent
Select 1-8.
In step (3) of the present invention, surfactant facilitates the surface for making lead ion equably be adsorbed on carbon.As excellent
Choosing, the surfactant are selected from least one of CTAB, PVP.CTAB, PVP of the present invention have in water
Good dissolubility is easy to separate with lead carbon composite (solid phase) in filtering or centrifugation.
Preferably, the mass ratio that feeds intake of the surfactant and carbon material is 0.1-10:1, more preferable 0.5-1:
1。
Preferably, the vacuum drying condition in step (3) are as follows: 60-80 DEG C vacuum drying 12-24 hours.
Preferably, the protective atmosphere be vacuum atmosphere or in argon gas, nitrogen, argon hydrogen gaseous mixture at least one
Kind.The more preferable protective atmosphere is argon hydrogen gaseous mixture.
Preferably, roasting described in step (4) uses temperature programming method, specifically: under protective atmosphere, presoma
1-6h is then kept the temperature to 300-700 DEG C by room temperature according to the heating rate of 1-8 DEG C/min.
On the other hand, the present invention provides nanometer lead/carbon composites as super lead carbon battery negative electrode active
The application of material.
Compared with prior art, the invention has the characteristics that and advantage:
1) the preparation method reduction of nanometer lead/carbon composite of the present invention carries out simultaneously with roasting, simpler in operation,
It is low in cost, it is not harsh to production equipment and condition；It obtained lead particle size minimum (50nm or less) and is evenly dispersed in
On the surface of carbon material.
2) the nanometer lead/carbon composite prepared is used as super lead carbon battery negative electrode active material, the lead of small-medium size
Particle can play the role of crystal seed in carbon material surface, and the lead sulfate particle formed during discharge is small, can be preferably
Delay the irreversible sulfation of cathode, and then improves the cycle life of super lead carbon battery.By surveying overpotential of hydrogen evolution discovery
Opposite carbon material itself has an increased 0.2-0.4V, illustrate that this lead/carbon composite can preferably inhibit evolving hydrogen reaction.
Detailed description of the invention
Fig. 1 is the scanning figure of 1 products therefrom of the invention patent embodiment,
Fig. 2 is the projection figure of 2 products therefrom of the invention patent embodiment,
Fig. 3 is the XRD diagram of 2 products therefrom of the invention patent embodiment,
Fig. 4 is the liberation of hydrogen test chart of 2 products therefrom of the invention patent embodiment.
Specific embodiment
Below by specific embodiment, technical scheme is described further, but protection scope of the present invention is not
It is limited to this:
In the embodiment of the present invention in the overpotential of hydrogen evolution of carbon material and specific capacitance test, the reference electrode of overpotential of hydrogen evolution is
The electrolyte of mercury/Mercurous sulfate electrode, specific capacitance test is the sulfuric acid solution of 1.28g/ml, is platinum electrode, reference electricity to electrode
Pole is mercury/Mercurous sulfate electrode.
Embodiment 1:
(1) it prepares solution 1: 10 ml deionized waters being added in 50 milliliters of beaker, 30% hydrogen peroxide 10 is then added
Milliliter, is stirred with glass bar, is uniformly mixed.
(2) it prepares solution 2: 1g coconut carbon (overpotential of hydrogen evolution 1.22V, specific capacitance are 160F/g) is added to solution 1
In, then in magnetic agitation half an hour.
(3) it prepares solution 3: 50 ml deionized waters is added in 250 milliliters of beakers, 1.655g plumbi nitras is then added,
Magnetic agitation half an hour.
(4) it prepares solution 4: solution 2 is added in solution 3, magnetic agitation half an hour.
(5) precursor preparation: 0.5gCTAB is added in solution 4, and magnetic agitation one hour, vacuum filtration, by solid
It is put into vacuum oven, is arranged 80 DEG C of temperature, drying time is 12 hours, obtains presoma.
(6) prepared by product: presoma grind into powder being put into tube furnace, setting program is as follows: initial temperature 25
DEG C, heating rate is 5 DEG C/min, and final temperature is 400 DEG C, keeps the temperature 2 hours, calcination atmosphere is nitrogen, is finally naturally cooling to
Room temperature finally obtains product.
(7) liberation of hydrogen is tested: this product 0.08g, PVDF 0.01g, acetylene black 0.01g are taken, is uniformly mixed in nmp solvent,
Slurry is made.Slurry is coated onto titanium sheet, obtains lead carbon resistance rod after dry；Coconut carbon is replaced into product, makes carbon electrode.With lead
Carbon resistance rod and carbon electrode make working electrode, and mercury/mereurous sulfate is auxiliary electrode, and platinum electrode is to electrode, and the sulfuric acid of 5mol/L is
Electrolyte, sweeping speed is 5mV/s, tests its hydrogen-evolution overpotential.The result shows that: overpotential of hydrogen evolution improves 0.23V after load nanometer lead,
Illustrate that this Nanometer sized lead oxide uniform load can preferably inhibit the evolving hydrogen reaction of carbon surface after carbon surface.
It can be seen that canescence protrusion particle is lead particle in SEM photograph in attached drawing 1, size is in 50nm hereinafter, seeing simultaneously
The surface of carbon is evenly distributed in lead.
Embodiment 2:
(1) solution 1: being added 20 ml deionized waters in 50 milliliters of beaker, and 10 milliliter of 30% hydrogen peroxide is then added,
It is stirred, is uniformly mixed with glass bar.
(2) solution 2: 0.1g rice hull carbon (overpotential of hydrogen evolution 1.2V, specific capacitance are 175F/g) is added in solution 1,
Then at magnetic agitation one hour.
(3) solution 3: being added 50 ml deionized waters in 250 milliliters of beakers, and 1g lead chloride, magnetic agitation is then added
One hour.
(4) solution 4: solution 2 is added in solution 3, magnetic agitation half an hour.
(5) precursor preparation: 0.1gPVP is added in solution 4, and magnetic agitation one hour, vacuum filtration put solid
Enter in vacuum oven, is arranged 80 DEG C of temperature, drying time is 12 hours.
(6) prepared by product: presoma grind into powder being put into tube furnace, setting program is as follows: initial temperature 25
DEG C, heating rate is 1 DEG C/min, and final temperature is 300 DEG C, keeps the temperature 1 hour, and calcination atmosphere is argon hydrogen gaseous mixture (argon gas: hydrogen
=95:5 (volume ratio)), it is finally naturally cooling to room temperature, finally obtains product.
(7) liberation of hydrogen is tested: this product 0.08g, PVDF 0.01g, acetylene black 0.01g are taken, is uniformly mixed in nmp solvent,
Slurry is made.Slurry is coated onto titanium sheet, obtains lead carbon resistance rod after dry；Rice hull carbon is replaced into product, makes carbon electrode.With lead
Carbon resistance rod and carbon electrode make working electrode, and mercury/mereurous sulfate is auxiliary electrode, and platinum electrode is to electrode, and the sulfuric acid of 5mol/L is
Electrolyte, sweeping speed is 5mV/s, tests its hydrogen-evolution overpotential.
It can be seen that white bright spot is lead particle in projection figure in attached drawing 2, size is in 50nm hereinafter, being evenly distributed.
It can be seen that the substance that XRD is loaded as the result is shown is lead in attached drawing 3.
It can be seen that the hydrogen-evolution overpotential of carbon material is -1.2V in attached drawing 4, and nanometer lead/carbon composite hydrogen-evolution overpotential
For -1.33V.Illustrate that this nanometer lead uniform load can preferably inhibit the evolving hydrogen reaction of carbon surface after carbon surface.
Embodiment 3:
(1) solution 1: being added 80 ml deionized waters in 250 milliliters of beaker, and 40 milliliter of 30% hydrogen peroxide is then added
It with 40 milliliters of nitric acid, is stirred, is uniformly mixed with glass bar.
(2) solution 2: by 1.0g graphene, (overpotential of hydrogen evolution 1.10V, specific capacitance are 202F/g.) it is added to solution 1
In, then at magnetic agitation one hour.
(3) solution 3: being added 50 ml deionized waters in 250 milliliters of beakers, and 5g lead acetate, magnetic agitation is then added
One hour.
(4) solution 4: solution 2 is added in solution 3, magnetic agitation half an hour.
(5) precursor preparation: 1gCTAB is added in solution 4, and magnetic agitation one hour, vacuum filtration put solid
Enter in vacuum oven, is arranged 80 DEG C of temperature, drying time is 12 hours.
(6) prepared by product: presoma grind into powder being put into tube furnace, setting program is as follows: initial temperature 25
DEG C, heating rate is 8 DEG C/min, and final temperature is 700 DEG C, keeps the temperature 6 hours, calcination atmosphere is argon gas, is finally naturally cooling to
Room temperature finally obtains product.
(7) liberation of hydrogen is tested: this product 0.08g, PVDF 0.01g, acetylene black 0.01g are taken, is uniformly mixed in nmp solvent,
Slurry is made.Slurry is coated onto titanium sheet, obtains lead carbon resistance rod after dry；Graphene is replaced into product, makes carbon electrode.With lead
Carbon resistance rod and carbon electrode make working electrode, and mercury/mereurous sulfate is auxiliary electrode, and platinum electrode is to electrode, and the sulfuric acid of 5mol/L is
Electrolyte, sweeping speed is 5mV/s, tests its hydrogen-evolution overpotential.The result shows that: overpotential of hydrogen evolution improves 0.24V after load nanometer lead,
Illustrate that this Nanometer sized lead oxide uniform load can preferably inhibit the evolving hydrogen reaction of carbon surface after carbon surface.
Embodiment 4:
(1) solution 1: being added 20 ml deionized waters in 50 milliliters of beaker, and it is dense that 10 milliliters of mass fractions are then added
The nitric acid that degree is 69%, is stirred with glass bar, is uniformly mixed.
(2) solution 2: 1.0g rice hull carbon (overpotential of hydrogen evolution 1.2V, specific capacitance are 175F/g) is added in solution 1,
Then at magnetic agitation one hour.
(3) solution 3: being added 50 ml deionized waters in 250 milliliters of beakers, and 1.655g plumbi nitras, magnetic force is then added
Stirring one hour.
(4) solution 4: solution 2 is added in solution 3, magnetic agitation half an hour.
(5) precursor preparation: 0.5gCTAB is added in solution 4, and magnetic agitation one hour, vacuum filtration, by solid
It is put into vacuum oven, is arranged 80 DEG C of temperature, drying time is 12 hours.
(6) prepared by product: presoma grind into powder being put into tube furnace, setting program is as follows: initial temperature 25
DEG C, heating rate is 4 DEG C/min, and final temperature is 550 DEG C, keeps the temperature 2 hours, calcination atmosphere is argon gas, is finally naturally cooling to
Room temperature finally obtains product.
(7) liberation of hydrogen is tested: this product 0.08g, PVDF 0.01g, acetylene black 0.01g are taken, is uniformly mixed in nmp solvent,
Slurry is made.Slurry is coated onto titanium sheet, obtains lead carbon resistance rod after dry；Rice hull carbon is replaced into product, makes carbon electrode.With lead
Carbon resistance rod and carbon electrode make working electrode, and mercury/mereurous sulfate is auxiliary electrode, and platinum electrode is to electrode, and the sulfuric acid of 5mol/L is
Electrolyte, sweeping speed is 5mV/s, tests its hydrogen-evolution overpotential.The result shows that: overpotential of hydrogen evolution improves 0.21V after load nanometer lead,
Illustrate that this Nanometer sized lead oxide uniform load can preferably inhibit the evolving hydrogen reaction of carbon surface after carbon surface.
Embodiment 5:
(1) solution 1: being added 20 ml deionized waters in 50 milliliters of beaker, and it is dense that 10 milliliters of mass fractions are then added
The nitric acid that degree is 69%, is stirred with glass bar, is uniformly mixed.
(2) solution 2: 1.0g coconut carbon (overpotential of hydrogen evolution 1.22V, specific capacitance are 160F/g) is added in solution 1,
Then at magnetic agitation one hour.
(3) solution 3: being added 50 ml deionized waters in 250 milliliters of beakers, and 1.655g plumbi nitras, magnetic force is then added
Stirring one hour.
(4) solution 4: solution 2 is added in solution 3, magnetic agitation half an hour.
(5) precursor preparation: 0.5gPVP is added in solution 4, and magnetic agitation one hour, vacuum filtration put solid
Enter in vacuum oven, is arranged 80 DEG C of temperature, drying time is 12 hours.
(6) prepared by product: presoma grind into powder being put into tube furnace, setting program is as follows: initial temperature 25
DEG C, heating rate is 4 DEG C/min, and final temperature is 550 DEG C, keeps the temperature 2 hours, calcination atmosphere is argon gas, is finally naturally cooling to
Room temperature finally obtains product.
(7) liberation of hydrogen is tested: this product 0.08g, PVDF 0.01g, acetylene black 0.01g are taken, is uniformly mixed in nmp solvent,
Slurry is made.Slurry is coated onto titanium sheet, obtains lead carbon resistance rod after dry；Coconut carbon is replaced into product, makes carbon electrode.With lead
Carbon resistance rod and carbon electrode make working electrode, and mercury/mereurous sulfate is auxiliary electrode, and platinum electrode is to electrode, and the sulfuric acid of 5mol/L is
Electrolyte, sweeping speed is 5mV/s, tests its hydrogen-evolution overpotential.The result shows that: overpotential of hydrogen evolution improves 0.18V after load nanometer lead,
Illustrate that this Nanometer sized lead oxide uniform load can preferably inhibit the evolving hydrogen reaction of carbon surface after carbon surface.
Claims (10)
1. a kind of nanometer of lead/carbon composite preparation method carries out in accordance with the following steps:
(1) carbon material is added in aqueous oxidizing agent solution and carries out oxidation processes, to improve the oxygen-containing functional group number of carbon material surface
Amount, obtains mixed liquor A；
(2) aqueous solution in lead source is mixed with mixed liquor A, stirring 0.5 hour or more, lead ion is made to be adsorbed on the table of carbon material
Face obtains mixed liquid B；
(3) surfactant is added into mixed liquid B, stirring 0.5 hour or more, then filtered, be dried in vacuo to obtain forerunner
Body；
(4) in protective atmosphere, to gained presoma carry out 300-700 DEG C roasting, obtained after heat treatment final product nanometer lead/
Carbon composite.
2. preparation method as described in claim 1, it is characterised in that: the carbon material is with high hydrogen-evolution overpotential and height electricity
Hold the carbon material of characteristic, wherein for overpotential of hydrogen evolution at least in 1.0V or more, reference electrode is mercury/Mercurous sulfate electrode)；Specific capacitance
At least in 150F/g or more, it is platinum electrode to electrode, reference electrode is that the electrolyte of test, which is the sulfuric acid solution of 1.28g/ml,
Mercury/Mercurous sulfate electrode.
3. preparation method as claimed in claim 2, it is characterised in that: the carbon material is selected from rice hull carbon, graphene, coconut husk
At least one of carbon.
4. the preparation method as described in one of claim 1-3, it is characterised in that: the oxidant is hydrogen peroxide and/or nitre
Acid.
5. preparation method as claimed in claim 4, it is characterised in that: the concentration of oxidant is 3- in aqueous oxidizing agent solution
30%；The volumetric usage of the aqueous oxidizing agent solution is calculated as 20-1600mL/g with the quality of carbon material.
6. the preparation method as described in one of claim 1-3, it is characterised in that: the lead source be selected from plumbi nitras, lead acetate,
At least one of lead chloride；The mass concentration of the aqueous solution in the lead source is 1.5-10%；The throwing in the lead source and carbon material
Material is than being calculated as 0.5-40, more preferable 1-8 with the mass ratio of lead and carbon material.
7. the preparation method as described in one of claim 1-3, it is characterised in that: the surfactant is selected from CTAB, PVP
At least one of；The mass ratio that feeds intake of the surfactant and carbon material is 0.1-10:1, more preferable 0.5-1:1.
8. the preparation method as described in one of claim 1-3, it is characterised in that: the protective atmosphere is vacuum atmosphere or choosing
From at least one of argon gas, nitrogen, argon hydrogen gaseous mixture.
9. the preparation method as described in one of claim 1-3, it is characterised in that: roasting described in step (4) uses program liter
Warm method, specifically: under protective atmosphere, presoma is according to the heating rate of 1-8 DEG C/min by room temperature to 300-700
DEG C, then keep the temperature 1-6h.
10. the lead of nanometer made from preparation method according to claim 1/carbon composite is as super lead carbon battery cathode
The application of active material.
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| CN103606656A (en) * | 2013-12-02 | 2014-02-26 | 华南师范大学 | Preparation method of lead oxide/graphene nanocomposite material for lead carbon super battery |
| CN107579240A (en) * | 2017-09-20 | 2018-01-12 | 吉林省凯禹电化学储能技术发展有限公司 | A kind of preparation method of C-base composte material for lead carbon battery negative pole |
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- 2018-12-16 CN CN201811538256.2A patent/CN109860531A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066248A (en) * | 2012-12-21 | 2013-04-24 | 中南大学 | Method for chemical doping of plumbum (Pb) on surface of cathode carbon material used for ultrabattery |
| CN103137955A (en) * | 2013-03-12 | 2013-06-05 | 深圳市雄韬电源科技股份有限公司 | Lead/carbon composite for storage battery and preparation method of lead/carbon composite material |
| CN103606656A (en) * | 2013-12-02 | 2014-02-26 | 华南师范大学 | Preparation method of lead oxide/graphene nanocomposite material for lead carbon super battery |
| CN107579240A (en) * | 2017-09-20 | 2018-01-12 | 吉林省凯禹电化学储能技术发展有限公司 | A kind of preparation method of C-base composte material for lead carbon battery negative pole |
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Application publication date: 20190607 |