CN105845929B - Preparation method of lead oxide-carbon composite material - Google Patents

Preparation method of lead oxide-carbon composite material Download PDF

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CN105845929B
CN105845929B CN201610370183.5A CN201610370183A CN105845929B CN 105845929 B CN105845929 B CN 105845929B CN 201610370183 A CN201610370183 A CN 201610370183A CN 105845929 B CN105845929 B CN 105845929B
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lead oxide
carbon
carbon composite
preparation
lead
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CN105845929A (en
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杨欢
邱于兵
郭兴蓬
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/56Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/56Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
    • H01M4/57Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead of "grey lead", i.e. powders containing lead and lead oxide
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a preparation method of a lead oxide-carbon composite material. The method comprises the following steps: (1) adding 300ml of 0.05-0.5M lead oxide precursor solution to each gram of carbon materials, mixing the lead oxide precursor solution and the carbon materials evenly, adjusting the pH value to be 8.5-9.0 and carrying out solid-phase drying after solid-liquid separation to obtain a raw material mixture; (2) burning the raw material mixture obtained in the step (1) at 500-800 DEG C in a protective gas atmosphere for 2 hours to obtain a lead oxide-carbon compound; and (3) adding the lead oxide-carbon compound obtained in the step (2) to 100ml of acid solution with the hydrogen ion content of 5M at 25-80 DEG C, fully washing and rinsing the product until the pH value is neutral and drying the product to prepare the lead oxide-carbon composite material. The method is simple; the operation is convenient; and by the compound synthesized by a high-temperature pyrolysis method and an acid-washing method, the micro-structure and the functional group on the surface are changed when PbO and the carbon material are compounded.

Description

A kind of preparation method of lead oxide-carbon composite
Technical field
The invention belongs to field of energy source materials, more particularly, to a kind of preparation method of lead oxide-carbon composite.
Background technology
Lead-acid battery the advantage such as is had a safety feature and is widely used in electrokinetic cell due to its low cost, technical maturity.But It is operated under high magnification partial state of charge (HRPSoC) can make negative terminal surface cover a large amount of irreversible PbSO4So as to reduce The utilization rate of active material, causes battery cycle life to reduce.It is that Carbon Materials are added in lead-acid battery cathode, using its height ratio Surface area, good electric conductivity and larger electric double layer capacitance improves the HRPSoC cycle lives of battery.
Chinese patent CN 102891285A disclose a kind of side of superbattery negative pole charcoal material surface chemical doping Pb Method, using strong affinities of the S and O to Pb and C, realizes Pb elements depth, uniform a large amount of doping in Carbon Materials microcosmos area, Carbon Materials liberation of hydrogen under so as to suppress acid system.
Although lead oxide-carbon composite prepared by this method has certain inhibition to liberation of hydrogen, but effect is still It is so not ideal enough.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of lead oxide-carbon composite Preparation method, its object is to increase the acidic functionality on lead oxide-carbon composite surface by pickling, thus solve existing Lead oxide-undesirable the technical problem of carbon composite liberation of hydrogen inhibition.
For achieving the above object, according to one aspect of the present invention, there is provided a kind of preparation of lead oxide-carbon composite Method, comprises the following steps:
(1) for every gram of Carbon Materials, lead oxide precursor solution 300ml for adding 0.05M to 0.5M uniformly mixes and adjusts Solid phase is dried to obtain raw mixture by section pH value between 8.5-9.0 after separation of solid and liquid;
(2) by the raw mixture obtained in step (1), 500 DEG C to 800 DEG C calcinings are obtained for 2 hours under protective gas atmosphere To lead oxide-Carbon composites;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in 5M at 25 DEG C to 80 DEG C Acid solution 100ml in fully wash, rinse to pH value in neutrality, be dried after i.e. be obtained the lead oxide-carbon composite.
Preferably, the preparation method of the lead oxide-carbon composite, its described Carbon Materials is activated carbon, carbon black, charcoal are received One or more in mitron, graphene oxide.
Preferably, the preparation method of the lead oxide-carbon composite, its described lead oxide precursor is lead (II) ion Solution.
Preferably, the preparation method of the lead oxide-carbon composite, its step (1) is adjusted using ammoniacal liquor or strong base solution Section pH value.
Preferably, the preparation method of the lead oxide-carbon composite, its step (3) temperature is 50 DEG C.
Preferably, the preparation method of the lead oxide-carbon composite, its described abundant washing concrete steps include:
Using stirring or ultrasonically treated 15 minutes to 5 hours.
Preferably, the preparation method of the lead oxide-carbon composite, its described abundant washing is concretely comprised the following steps:
Acid solution is processed 30 minutes and changed using magnetic agitation, repeats operation 3 times above.
Preferably, the preparation method of the lead oxide-carbon composite, its described abundant washing is concretely comprised the following steps:
Using ultrasonically treated 15 minutes.
According to another aspect of the present invention, there is provided a kind of lead oxide-carbon composite, it is characterised in that according to such as It is prepared by the method described in claim 1 to 8 any one.
In general, by the contemplated above technical scheme of the present invention compared with prior art, can obtain down and show Beneficial effect:
The inventive method is simple, easy to operate, the compound synthesized using high temperature pyrolysis and acid wash, in PbO and raw material of wood-charcoal While material is compound, the functional group on its micro-structural and surface is changed.Most of PbO that its pickling is dissolved away plays " pore creating material " work With the pore volume for making composite increases, and hole number increases, while the acidic functionality that charcoal material surface increases is easy to active lead In surface deposition, suppress Carbon Materials liberation of hydrogen under acid system;Uniformly absorption, on C-material surface, improves negative pole to another aspect PbO Lead charcoal adhesion in active material, increases the overpotential of hydrogen evolution of electrode, so as to substantially reduce charcoal material surface liberation of hydrogen, while gram Take the proportion of Carbon Materials and the inconsistence problems of lead so as to be well mixed between active material, improve its HRPSoC circulation longevity Life.It is suitable to industrial applications.
Description of the drawings
Fig. 1 is the compound ESEM and energy spectrum diagram of the high temperature pyrolysis-high temperature acid wash of embodiment 2 synthesis;Wherein Fig. 1 A () is the scanning electron microscope (SEM) photograph of Pb-C-50 DEG C of pickling compound;Fig. 1 (b) and (c) are respectively Pb-C-50 DEG C of pickling composite particles The distribution of surface Pb elements and O elements;
Curve 1,2,3,4,5,6 in Fig. 2 is respectively blank negative pole in embodiment 1, example 2 and comparative example and different compound During thing (carbon black, Pb-C-500 DEG C of calcining, Pb-C-25 DEG C of pickling, Pb-C-50 DEG C of pickling and C-50 DEG C of pickling) is added to negative pole Cathodic polarization curve;
Fig. 3 be the hollow white appliances pond of embodiment 1, example 2 and comparative example and different compound (carbon black, Pb-C-500 DEG C of calcining, Pb-C-25 DEG C of pickling, Pb-C-50 DEG C of pickling and C-50 DEG C of pickling) it is added in electrode and is assembled into battery under HRPSoC states Cycle life curve;
Curve 1,2,3,4 in Fig. 4 is respectively blank negative pole and different compound (GO, Pb-GO-500 in embodiment 5 DEG C calcining, Pb-GO- ultrasound pickling) cathodic polarization curve that is added in negative pole;
Fig. 5 is the hollow white appliances pond of embodiment 5 and different compound (GO, Pb-GO-500 DEG C of calcining, Pb-GO- ultrasound acid Wash) it is added in electrode the cycle life curve for being assembled into battery under HRPSoC states.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and It is not used in the restriction present invention.As long as additionally, technical characteristic involved in invention described below each embodiment Not constituting conflict each other just can be mutually combined.
The preparation method of lead oxide-carbon composite that the present invention is provided, comprises the following steps:
(1) for every gram of Carbon Materials, lead oxide precursor solution 300ml for adding 0.05M to 0.5M uniformly mixes and adjusts Solid phase is dried to obtain raw mixture by section pH value between 8.5-9.0 after separation of solid and liquid;
The Carbon Materials are one or more in activated carbon, carbon black, carbon nanotube, graphene oxide;The lead oxide Precursor be lead (II) ion solution, such as lead nitrate solution, acetic acid lead solution;Adjusting pH value can be molten using ammoniacal liquor or highly basic Liquid, such as potassium hydroxide solution, sodium hydroxide solution.
(2) by the raw mixture obtained in step (1), 500 DEG C to 800 DEG C calcinings are obtained for 2 hours under protective gas atmosphere To lead oxide-Carbon composites;
(3) lead oxide-Carbon composites that will be obtained in step (2), at 25 DEG C to 80 DEG C, at preferably 50 DEG C hydrogen ion are added Content is fully washed in the acid solution 100ml of 5M, is rinsed to pH value in neutrality, and the lead oxide-charcoal is obtained after being dried Composite.
Preferably, the abundant washing concrete steps include:Using stirring or it is ultrasonically treated 15 minutes to 5 hours, specifically Ground, when using magnetic agitation, processes 30 minutes and changes acid solution, repeats operation 3 times above;When using ultrasound, place Reason 15 minutes.
Lead oxide-carbon composite that the present invention is provided, prepares according to the method described above.
It is below embodiment:
Embodiment 1
A kind of preparation method of lead oxide-carbon composite, comprises the following steps:
(1) for every gram of Carbon Materials, lead nitrate solution 300ml for adding 0.05M uniformly mixes and adjusts pH value in 8.5- Between 9.0, solid phase is dried to obtain into raw mixture after separation of solid and liquid;
The Carbon Materials are carbon black;The lead oxide precursor is lead nitrate solution;Adjust pH value and adopt ammoniacal liquor.
(2) by the raw mixture obtained in step (1), under a nitrogen 500 DEG C of calcinings obtain lead oxide-charcoal for 2 hours and are combined Thing;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in the hydrochloric acid of 5M at 25 DEG C Fully wash in solution 100ml, rinse to pH value in neutrality, the lead oxide-carbon composite is obtained after being dried.
Fully washing is comprised the following steps that:Acid solution is processed 30 minutes and changed using magnetic agitation, repeats to grasp above Make 3 times.
Lead oxide-the carbon composite, carbon black and Pb-C-500 DEG C are calcined the compound for obtaining, work is respectively added to In industry lead plaster, the lead plaster of certain mass is applied into exhibition on stereotype grid, according to the solidification of existing industrial procedure, chemical conversion after being well mixed After obtain lead-acid battery cathode plate.
Cathodic polarization curve test is carried out on electrochemical workstation using three-electrode system, test solution is 5mol/L H2SO4, different compounds (carbon black, lead oxide-carbon composite that Pb-C-500 DEG C of calcining and the present embodiment are provided) are added to Test curve in negative pole adds the hydrogen-evolution overpotential size order of different composite thing rear electrode as shown in the curve 2,3,4 in Fig. 2 For:Carbon black (﹣ 1.218V)>Blank (﹣ 1.228V)>Pb-C-500 DEG C of calcining (﹣ 1.253V)>The lead oxide that the present embodiment is provided- Carbon composite (﹣ 1.296V), the compound after as a result explanation calcining and normal temperature pickling is added to the hydrogen-evolution overpotential ratio in negative pole Blank negative pole and other addition cathode composites it is more negative, relative to blank and addition carbon black electrode, its liberation of hydrogen electric current reduces.
By above-mentioned different compound (carbon black, lead oxide-charcoal composite wood that Pb-C-500 DEG C of calcining and the present embodiment are provided Material) negative pole is respectively added to, according to " two positive one is negative " battery is assembled into, using 2C charging 30s, 10s, 2C electric discharge 30s are shelved, Shelve the circulating process of 10s carries out discharge and recharge to it, and its cycle life curve is as shown in figure 3, add battery after different composite thing Cycle life size order be:Lead oxide-carbon composite that the present embodiment is provided>Carbon black>It is blank>Pb-C-500 DEG C is forged Burn, the compound after as a result explanation calcining and normal temperature pickling is added in negative pole and is added to electricity than blank battery and other compounds The cycle life in pond is longer.
Embodiment 2
A kind of preparation method of lead oxide-carbon composite, comprises the following steps:
(1) for every gram of Carbon Materials, lead nitrate solution 300ml for adding 0.05M uniformly mixes and adjusts pH value in 8.5- Between 9.0, solid phase is dried to obtain into raw mixture after separation of solid and liquid;
The Carbon Materials are carbon black;The lead oxide precursor is lead nitrate solution;Adjust pH value and adopt ammonia spirit.
(2) by the raw mixture obtained in step (1), under a nitrogen 500 DEG C of calcinings obtain lead oxide-charcoal for 2 hours and are combined Thing;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in the hydrochloric acid of 5M at 50 DEG C Fully wash in solution 100ml, rinse to pH value in neutrality, the lead oxide-carbon composite is obtained after being dried.
Fully washing is comprised the following steps that:Acid solution is processed 30 minutes and changed using magnetic agitation, repeats to grasp above Make 3 times.
Lead oxide-charcoal that the SEM figures of lead oxide-carbon composite that Fig. 1 is provided for the present embodiment and the present embodiment are provided The energy spectrum diagram of composite material granular.It can be seen that lead oxide-carbon composite even particle size that the present embodiment is provided, and Pb Element is evenly distributed on C particle surfaces with O elements.
Lead oxide-carbon composite that the present embodiment is provided is added in industrial lead plaster, will be certain after being well mixed The lead plaster of quality applies exhibition on stereotype grid, and according to the solidification of existing industrial procedure, after being melted into lead-acid battery cathode plate is obtained.
Cathodic polarization curve test is carried out on electrochemical workstation using three-electrode system, test solution is 5mol/L H2SO4, its test curve compares other additives as shown in the curve 5 in Fig. 2, add lead oxide that the present embodiment provides- Current potential before the hydrogen-evolution overpotential (﹣ 1.333V) of negative pole is than adding after carbon composite is more negative, and liberation of hydrogen speed reduces.
Lead oxide-carbon composite that the present embodiment is provided is added in negative pole and is assembled into " two positive one is negative " battery, adopted With 2C charging 30s, 10s, 2C electric discharge 30s are shelved, shelve the circulating process of 10s carries out discharge and recharge to it, its cycle life curve As shown in figure 3, add the present embodiment provide lead oxide-carbon composite after battery cycle life increase it is most.
Embodiment 3
A kind of preparation method of lead oxide-carbon composite, comprises the following steps:
(1) for every gram of Carbon Materials, the acetic acid lead solution 300ml for adding 0.5M uniformly mixes and adjusts pH value in 8.5- Between 9.0, solid phase is dried to obtain into raw mixture after separation of solid and liquid;
The Carbon Materials are carbon nanotube;The lead oxide precursor is lead acetate;Adjust pH value molten using potassium hydroxide Liquid.
(2) by the raw mixture obtained in step (1), under argon gas 800 DEG C of calcinings obtain lead oxide-charcoal for 2 hours and are combined Thing;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in the nitric acid of 5M at 80 DEG C Fully wash in solution 100ml, rinse to pH value in neutrality, the lead oxide-carbon composite is obtained after being dried.
Fully washing is comprised the following steps that:Using ultrasonically treated 15 minutes.
Embodiment 4
A kind of preparation method of lead oxide-carbon composite, comprises the following steps:
(1) for every gram of Carbon Materials, the acetic acid lead solution 300ml for adding 0.1M uniformly mixes and adjusts pH value in 8.5- Between 9.0, solid phase is dried to obtain into raw mixture after separation of solid and liquid;
The Carbon Materials are activated carbon;The lead oxide precursor is acetic acid lead solution;Adjust pH value and adopt NaOH Solution.
(2) by the raw mixture obtained in step (1), under argon gas 650 DEG C of calcinings obtain lead oxide-charcoal for 2 hours and are combined Thing;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in the sulfuric acid of 5M at 50 DEG C Fully wash in solution 100ml, rinse to pH value in neutrality, the lead oxide-carbon composite is obtained after being dried.
Fully washing is comprised the following steps that:Acid solution is processed 30 minutes and changed using magnetic agitation, repeats to grasp above Make 3 times.
Embodiment 5
A kind of preparation method of lead oxide-carbon composite, comprises the following steps:
(1) for every gram of Carbon Materials, lead nitrate solution 300ml for adding 0.05M uniformly mixes and adjusts pH value in 8.5- Between 9.0, solid phase is dried to obtain into raw mixture after separation of solid and liquid;
The Carbon Materials are graphene oxide;The lead oxide precursor is plumbi nitras;Adjust pH value and adopt ammoniacal liquor.
(2) by the raw mixture obtained in step (1), under a nitrogen 500 DEG C of calcinings obtain lead oxide-charcoal for 2 hours and are combined Thing;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in the hydrochloric acid of 5M at 25 DEG C Fully wash in solution 100ml, rinse to pH value in neutrality, the lead oxide-carbon composite is obtained after being dried.
Fully washing is comprised the following steps that:Using ultrasonically treated 15 minutes.
By the compound after different disposal, (lead oxide-charcoal that GO, Pb-GO-500 DEG C of calcining and the present embodiment are provided is combined Thing) industrial lead plaster is respectively added to, the lead plaster of certain mass is applied into exhibition on the stereotype grid, according to existing work after being well mixed Lead-acid battery cathode plate is obtained after industry program Solidification, chemical conversion.
Cathodic polarization curve test is carried out on electrochemical workstation using three-electrode system, test solution is 5mol/L H2SO4.Its test curve adds the hydrogen-evolution overpotential size order of different composite thing rear electrode as shown in the curve 2,3,4 in Fig. 4 For:Blank (﹣ 1.228V)>GO (﹣ 1.247V)>Pb-GO-500 DEG C of calcining (﹣ 1.270V)>Lead oxide-charcoal that the present embodiment is provided Compound after compound, as a result explanation calcining and ultrasonic pickling is added in negative pole and is added to relative to GO and other additives Hydrogen-evolution overpotential in negative pole is more negative, is added to its liberation of hydrogen electric current in negative pole relative to GO and reduces.
By above-mentioned different compound (lead oxide-Carbon composites that GO, Pb-GO-500 DEG C of calcining and the present embodiment are provided) It is respectively added to be assembled into " two positive one is negative " battery in negative pole, using 2C charging 30s, shelves 10s, 2C electric discharge 30s, shelves 10s Circulating process discharge and recharge is carried out to it, its cycle life curve as shown in figure 5, add different composite thing after battery the circulation longevity Ordering size order is:Lead oxide-Carbon composites that the present embodiment is provided>GO>It is blank>Pb-GO-500 DEG C of calcining, as a result explanation is forged Compound is added in negative pole the cycle life that can dramatically increase battery after burning and ultrasonic pickling.
Comparative example
By carbon black dispersion magnetic agitation 2h in ethanol, NH is added dropwise3·H2O and ultrasonically treated 10min, filtering vacuum is dried, This material is calcined into 2h in 500 DEG C of nitrogen atmospheres, C-500 DEG C of calcining of simple substance is obtained.To C-500 DEG C after high-temperature calcination in 5M 50 DEG C of pickling are carried out in HCl, C-50 DEG C of pickling of simple substance is obtained.
C-50 DEG C of pickling of simple substance is added in industrial lead plaster, the lead plaster of certain mass is applied into exhibition to lead after being well mixed On grid, according to the solidification of existing industrial procedure, after being melted into lead-acid battery cathode plate is obtained.
Cathodic polarization curve test is carried out on electrochemical workstation using three-electrode system, test solution is 5mol/L H2SO4, as shown in the curve 6 in Fig. 2, its hydrogen-evolution overpotential (﹣ 1.315V) is than adding Pb-C-50 DEG C of pickling compound for test curve Afterwards the hydrogen-evolution overpotential (﹣ 1.333V) of negative pole just, but adds the hydrogen-evolution overpotential of negative poles more negative relative to other compounds, liberation of hydrogen speed It is less after than adding Pb-C-50 DEG C of pickling compound, illustrate that C-50 DEG C of pickling is added in negative pole the analysis that can suppress negative pole Hydrogen.
Above-mentioned C-50 DEG C of pickling compound is added in negative pole and is assembled into " two positive one is negative " battery, using 2C charging 30s, puts 10s, 2C electric discharge 30s are put, shelve the circulating process of 10s carries out discharge and recharge to it, and its cycle life curve is as shown in Figure 3.Simple substance The cycle life that C-50 DEG C of pickling is added to battery in negative pole is most short.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not to The present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc. are limited, all should be included Within protection scope of the present invention.

Claims (9)

1. a kind of preparation method of lead oxide-carbon composite, it is characterised in that comprise the following steps:
(1) for every gram of Carbon Materials, lead oxide precursor solution 300ml for adding 0.05M to 0.5M uniformly mixes and adjusts pH Solid phase is dried to obtain raw mixture by value between 8.5-9.0 after separation of solid and liquid;
(2) by the raw mixture obtained in step (1), 500 DEG C to 800 DEG C calcinings obtain oxygen in 2 hours under protective gas atmosphere Change lead-Carbon composites;
(3) lead oxide-Carbon composites that will be obtained in step (2), add hydrogen ion content in the salt of 5M at 25 DEG C to 80 DEG C Fully wash in acid solution 100ml, rinse to pH value in neutrality, the lead oxide-carbon composite is obtained after being dried.
2. the preparation method of lead oxide-carbon composite as claimed in claim 1, it is characterised in that the Carbon Materials are to live One or more in property charcoal, carbon black, carbon nanotube, graphene oxide.
3. the preparation method of lead oxide-carbon composite as claimed in claim 1, it is characterised in that body before the lead oxide Body is lead (II) ion solution.
4. the preparation method of lead oxide-carbon composite as claimed in claim 1, it is characterised in that step (1) adopts ammoniacal liquor Or strong base solution adjusts pH value.
5. the preparation method of lead oxide-carbon composite as claimed in claim 1, it is characterised in that step (3) temperature is 50 ℃。
6. the preparation method of lead oxide-carbon composite as claimed in claim 1, it is characterised in that the abundant washing tool Body step includes:
Using stirring or ultrasonically treated 15 minutes to 5 hours.
7. the preparation method of lead oxide-carbon composite as claimed in claim 6, it is characterised in that the abundant washing tool Body step is:
Acid solution is processed 30 minutes and changed using magnetic agitation, repeats operation 3 times above.
8. the preparation method of lead oxide-carbon composite as claimed in claim 6, it is characterised in that the abundant washing tool Body step is:
Using ultrasonically treated 15 minutes.
9. a kind of lead oxide-carbon composite, it is characterised in that according to the method system as described in claim 1 to 8 any one It is standby.
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CN108393082B (en) * 2018-03-06 2020-12-01 淮南市通霸蓄电池有限公司 Nano lead oxide-carbon composite material and preparation method thereof
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