CN106025197A - Preparation method of carbon-coated lead powder composite for lead-carbon battery - Google Patents
Preparation method of carbon-coated lead powder composite for lead-carbon battery Download PDFInfo
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- CN106025197A CN106025197A CN201610330237.5A CN201610330237A CN106025197A CN 106025197 A CN106025197 A CN 106025197A CN 201610330237 A CN201610330237 A CN 201610330237A CN 106025197 A CN106025197 A CN 106025197A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/56—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
- H01M4/57—Selection 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
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 relates to a preparation method of a carbon-coated lead powder composite for a lead-carbon battery. An organic carbon source is substituted for a common active carbon material in the prior art, and sol is adopted as a precursor, so that the surface of lead powder is evenly coated with carbon, and the super capacitor characteristic of a carbon material can be effectively realized; the carbon material is dried and granulated with a spray granulation technology to form the fine and even carbon-coated lead powder composite, the problem of uneven mixing of the lead powder and the carbon source is solved, reduction of the mechanical strength of the composite due to accumulation of lead sulfate salt and traditional mechanical grinding is prevented, the reaction activity of a battery cathode can be effectively enhanced, and the reaction efficiency is improved; mist particles ranging from 100 mu m to 200 mu m polymerized with the spray granulation technology are directly contacted with hot air, the surface area is greatly increased, 95%-98% of moisture can be evaporated in high-temperature air flow, drying is completed, processes such as evaporation, grinding and the like in the prior art can be omitted, steps are simplified, and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of carbon for lead carbon battery and be coated with the spray drying preparation of powder composite.
Background technology
In existing lead carbon battery, material with carbon element all adds in the lead plaster of lead carbon battery in the way of mechanical mixture with Hydrocerussitum (Ceruse), with
The carrying out of charge and discharge process, lead can produce huge change in volume with lead sulfate when converting, and the great variety of volume is produced
Raw stress necessarily causes Hydrocerussitum (Ceruse) to lose the parcel of powdered carbon and dissociates in electrolyte even in dividing plate space, causes battery short
Road.Meanwhile, more than 2% in the Hydrocerussitum (Ceruse) of powdered carbon addition and powdered carbon mixture, powdered carbon proportion is relatively big, causes lead
Between powder particles, contact point reduces, and the corrosive bond effect between Hydrocerussitum (Ceruse) and Hydrocerussitum (Ceruse) declines, the more conventional pole plate of intensity of pole plate
Difference is very big, and pole plate is easy to lose conductive capability in cyclic process, and causes battery life to reduce rapidly.
Application publication number is Chinese invention patent application " a kind of lead carbon composite electro-deposition dress of CN103952747A
Put " (application number: CN201410147584.5) refer to a kind of electro-deposition techniques, and it is to activated carbon by lead deposit
Space between intragranular portion and activated carbon granule is to prepare lead carbon composite.This method can only be plated in the one side of carbon coating
Lead, and lead layer can not be completely covered charcoal particle surface；Meanwhile, the method needs the activated carbon coating of lead plating from motherboard
On scrape, cause the mechanical strength properties of composite to be nowhere near, the mixing uniformity of lead carbon is not enough.
Authorization Notice No. is Chinese invention patent " a kind of carbon cladding for lead carbon superbattery of CN102637858B
The microwave preparation of powder composite " (application number: CN201210070245.2) refer to a kind of coating technology,
It is to use microwave carbonization process, washing to be dried to obtain lead carbon composite, but, the method does not ensure that carbon is coated with lead
The grain size of composite, and again after mechanical activation comminution processes, the lead of charcoal particle surface can be destroyed damage further,
The mixing uniformity that still can cause lead carbon is poor.
The lead plaster that above-mentioned existing Hydrocerussitum (Ceruse) and carbon source mixing make is extremely difficult to the technology requirement of lead carbon battery negative pole, and lead carbon mixes
Closing uneven so that cell reaction efficiency is low, cause battery charging and discharging not thorough, battery is low.Therefore, right
It is coated with the preparation method of powder composite in the carbon for lead carbon battery, awaits further being improved.
Summary of the invention
The technical problem to be solved is the present situation for prior art, it is provided that one can be effectively improved the mixing of lead carbon
The carbon for lead carbon battery of uniformity is coated with the preparation method of powder composite.
The present invention solves the technical scheme that above-mentioned technical problem used: it is multiple that a kind of carbon for lead carbon battery is coated with Hydrocerussitum (Ceruse)
The preparation method of condensation material, it is characterised in that comprise the following steps:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, Hydrocerussitum (Ceruse) is mixed to get with deionized water
Mixed liquid B；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, this mixed liquor C is added hydro-thermal
In reactor, at 160～200 DEG C, disperse 10～12h；
(2) take out the mixed liquor C in hydrothermal reaction kettle, remove the supernatant, obtain colloidal sol D；Utilize and be spray-dried
Machine carries out mist projection granulating to this colloidal sol D；
(3) under inert gas shielding, the granule that step (2) obtains is carried out carbonization so that granular active carbon is reunited
The carbon source pyrolysis of surface forms pyrolytic carbon；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is placed in true after washing
Empty drying baker is dried 6～10h, i.e. obtains the described carbon for lead carbon battery and be coated with powder composite.
In such scheme, described in step (1), glucose with the gross weight of sucrose with the weight ratio of deionized water is
1:(4～50).
Hydrocerussitum (Ceruse) described in step (1) is 1:(2.5～4 with the weight ratio of deionized water).
Glucose described in step (1) and the gross weight of sucrose are (2～12) with the weight ratio of Hydrocerussitum (Ceruse): 100.
As preferably, a diameter of 100～200 μm of mist projection granulating gained granule in step (2).
Preferably, in step (2), mist projection granulating uses atomizer pelletize, and centrifugal rotational speed is 120～400r/min,
Temperature is 50～90 DEG C.
In above-mentioned each preferred version, in step (3), constant temperature carburizing temperature is 400～600 DEG C, and carbonization time is 2～6
h。
In step (4), baking temperature is 40～60 DEG C, and vacuum is 20～100kPa.
Compared with prior art, it is an advantage of the current invention that:
The present invention uses organic carbon source to replace absorbent charcoal material commonly used in the prior art, by mixing, mist projection granulating, carbon
Change, washing drying and other steps is prepared for carbon cladding powder composite, and presoma uses colloidal sol so that carbon is evenly coated at
The surface of Hydrocerussitum (Ceruse), it is possible to effectively play the supercapacitor properties of material with carbon element；Be allowed to be dried by spray granulation, pelletize
Become the carbon cladding powder composite of fine uniform, solve Hydrocerussitum (Ceruse), the carbon source uneven problem of mixing, it is to avoid sulphuric acid
The problem of the decline causing composite machinery intensity is pulverized in the accumulation of lead salt, traditional mechanical, can effectively strengthen battery cathode
Reactivity, improve reaction efficiency, extend lead carbon battery service life cycle；
The present invention utilizes spray granulation dimerization to become the vaporific microgranule of 100～200 μm directly to contact with hot-air, table
Area is greatly increased, and can evaporate the moisture content of 95%～98% in high temperature gas flow, completes to be dried, and can save in prior art
Evaporation, the operation such as pulverizing, simplify step, reduce production cost.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
The present embodiment comprises the following steps for the preparation method of the carbon cladding powder composite of lead carbon battery:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, the gross weight of glucose and sucrose with go
The weight ratio of ionized water is 1:4；Hydrocerussitum (Ceruse) and deionized water are mixed to get the weight of mixed liquid B, Hydrocerussitum (Ceruse) and deionized water
The ratio of amount is 1:2.5；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, and make Portugal in mixed liquor C
Grape sugar and the gross weight of sucrose are 2:100 with the weight ratio of Hydrocerussitum (Ceruse)；This mixed liquor C is added in hydrothermal reaction kettle, in
12h is disperseed at 160 DEG C；
(2) take out the mixed liquor C in hydrothermal reaction kettle, use separatory funnel to remove the supernatant, obtain colloidal sol D；
Utilizing centrifugal spray dryer that this colloidal sol D is carried out mist projection granulating, centrifugal rotational speed is 120r/min, and temperature is 90 DEG C,
About a diameter of 100 μm of gained granule；
(3) under inert gas shielding, the granule that step (2) obtains being carried out constant temperature carbonization, carburizing temperature is 400
DEG C, carbonization time is 6h so that the carbon source pyrolysis on granular active carbon aggregate surface forms pyrolytic carbon, strengthens aggregate
Structural strength, improve the conductive capability of activated carbon aggregate；
(4) with ethanol and deionized water, the granule that step (3) obtains alternately is washed 3 times, granulated pellet is existed
Other impurity produced during forming pyrolytic carbon washes, and is placed in vacuum drying oven and is dried 6h after washing, dry
Dry temperature is 60 DEG C, and vacuum is 100kPa, obtains the carbon for lead carbon battery and is coated with powder composite.
Embodiment 2:
The present embodiment comprises the following steps for the preparation method of the carbon cladding powder composite of lead carbon battery:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, the gross weight of glucose and sucrose with go
The weight ratio of ionized water is 1:50；Hydrocerussitum (Ceruse) and deionized water are mixed to get mixed liquid B, Hydrocerussitum (Ceruse) and deionized water
Weight ratio is 1:4；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, and make in mixed liquor C
Glucose and the gross weight of sucrose are 12:100 with the weight ratio of Hydrocerussitum (Ceruse)；This mixed liquor C is added in hydrothermal reaction kettle,
10h is disperseed at 200 DEG C；
(2) take out the mixed liquor C in hydrothermal reaction kettle, use separatory funnel to remove the supernatant, obtain colloidal sol D；
Utilizing centrifugal spray dryer that this colloidal sol D is carried out mist projection granulating, centrifugal rotational speed is 400r/min, and temperature is 50 DEG C,
About a diameter of 200 μm of gained granule；
(3) under inert gas shielding, the granule that step (2) obtains being carried out constant temperature carbonization, carburizing temperature is 600
DEG C, carbonization time is 2h so that the carbon source pyrolysis on granular active carbon aggregate surface forms pyrolytic carbon, strengthens aggregate
Structural strength, improve the conductive capability of activated carbon aggregate；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is being formed by granulated pellet
Other impurity produced during pyrolytic carbon washes, and is placed in vacuum drying oven and is dried 10h after washing, is dried temperature
Degree is 40 DEG C, and vacuum is 20kPa, obtains the carbon for lead carbon battery and is coated with powder composite.
Embodiment 3:
The present embodiment comprises the following steps for the preparation method of the carbon cladding powder composite of lead carbon battery:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, the gross weight of glucose and sucrose with go
The weight ratio of ionized water is 1:4；Hydrocerussitum (Ceruse) and deionized water are mixed to get the weight of mixed liquid B, Hydrocerussitum (Ceruse) and deionized water
The ratio of amount is 1:4；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, and make Portugal in mixed liquor C
Grape sugar and the gross weight of sucrose are 5:100 with the weight ratio of Hydrocerussitum (Ceruse)；This mixed liquor C is added in hydrothermal reaction kettle, in
11h is disperseed at 180 DEG C；
(2) take out the mixed liquor C in hydrothermal reaction kettle, use separatory funnel to remove the supernatant, obtain colloidal sol D；
Utilizing centrifugal spray dryer that this colloidal sol D is carried out mist projection granulating, centrifugal rotational speed is 200r/min, and temperature is 60 DEG C,
About a diameter of 150 μm of gained granule；
(3) under inert gas shielding, the granule that step (2) obtains being carried out constant temperature carbonization, carburizing temperature is 500
DEG C, carbonization time is 3h so that the carbon source pyrolysis on granular active carbon aggregate surface forms pyrolytic carbon, strengthens aggregate
Structural strength, improve the conductive capability of activated carbon aggregate；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is being formed by granulated pellet
Other impurity produced during pyrolytic carbon washes, and is placed in vacuum drying oven and is dried 7h after washing, is dried temperature
Degree is 50 DEG C, and vacuum is 100kPa, obtains the carbon for lead carbon battery and is coated with powder composite.
Embodiment 4:
The present embodiment comprises the following steps for the preparation method of the carbon cladding powder composite of lead carbon battery:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, the gross weight of glucose and sucrose with go
The weight ratio of ionized water is 1:50；Hydrocerussitum (Ceruse) and deionized water are mixed to get mixed liquid B, Hydrocerussitum (Ceruse) and deionized water
Weight ratio is 1:2.5；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, and make in mixed liquor C
Glucose and the gross weight of sucrose are 12:100 with the weight ratio of Hydrocerussitum (Ceruse)；This mixed liquor C is added in hydrothermal reaction kettle,
11h is disperseed at 200 DEG C；
(2) take out the mixed liquor C in hydrothermal reaction kettle, use separatory funnel to remove the supernatant, obtain colloidal sol D；
Utilizing centrifugal spray dryer that this colloidal sol D is carried out mist projection granulating, centrifugal rotational speed is 300r/min, and temperature is 80 DEG C,
A diameter of 100 μm of gained granule；
(3) under inert gas shielding, the granule that step (2) obtains being carried out constant temperature carbonization, carburizing temperature is 500
DEG C, carbonization time is 5h so that the carbon source pyrolysis on granular active carbon aggregate surface forms pyrolytic carbon, strengthens aggregate
Structural strength, improve the conductive capability of activated carbon aggregate；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is being formed by granulated pellet
Other impurity produced during pyrolytic carbon washes, and is placed in vacuum drying oven and is dried 7h after washing, is dried temperature
Degree is 60 DEG C, and vacuum is 50kPa, obtains the carbon for lead carbon battery and is coated with powder composite.
Embodiment 5:
The present embodiment comprises the following steps for the preparation method of the carbon cladding powder composite of lead carbon battery:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, the gross weight of glucose and sucrose with go
The weight ratio of ionized water is 1:20；Hydrocerussitum (Ceruse) and deionized water are mixed to get mixed liquid B, Hydrocerussitum (Ceruse) and deionized water
Weight ratio is 1:3；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, and make in mixed liquor C
Glucose and the gross weight of sucrose are 6:100 with the weight ratio of Hydrocerussitum (Ceruse)；This mixed liquor C is added in hydrothermal reaction kettle,
12h is disperseed at 160 DEG C；
(2) take out the mixed liquor C in hydrothermal reaction kettle, use separatory funnel to remove the supernatant, obtain colloidal sol D；
Utilizing centrifugal spray dryer that this colloidal sol D is carried out mist projection granulating, centrifugal rotational speed is 120r/min, and temperature is 80 DEG C,
About a diameter of 120 μm of gained granule；
(3) under inert gas shielding, the granule that step (2) obtains being carried out constant temperature carbonization, carburizing temperature is 600
DEG C, carbonization time is 3h so that the carbon source pyrolysis on granular active carbon aggregate surface forms pyrolytic carbon, strengthens aggregate
Structural strength, improve the conductive capability of activated carbon aggregate；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is being formed by granulated pellet
Other impurity produced during pyrolytic carbon washes, and is placed in vacuum drying oven and is dried 8h after washing, is dried temperature
Degree is 55 DEG C, and vacuum is 60kPa, obtains the carbon for lead carbon battery and is coated with powder composite.
Embodiment 6:
The present embodiment comprises the following steps for the preparation method of the carbon cladding powder composite of lead carbon battery:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, the gross weight of glucose and sucrose with go
The weight ratio of ionized water is 1:25；Hydrocerussitum (Ceruse) and deionized water are mixed to get mixed liquid B, Hydrocerussitum (Ceruse) and deionized water
Weight ratio is 1:4；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, and make in mixed liquor C
Glucose and the gross weight of sucrose are 7:100 with the weight ratio of Hydrocerussitum (Ceruse)；This mixed liquor C is added in hydrothermal reaction kettle,
10h is disperseed at 180 DEG C；
(2) take out the mixed liquor C in hydrothermal reaction kettle, use separatory funnel to remove the supernatant, obtain colloidal sol D；
Utilizing centrifugal spray dryer that this colloidal sol D is carried out mist projection granulating, centrifugal rotational speed is 200r/min, and temperature is 70 DEG C,
About a diameter of 110 μm of gained granule；
(3) under inert gas shielding, the granule that step (2) obtains being carried out constant temperature carbonization, carburizing temperature is 600
DEG C, carbonization time is 5h so that the carbon source pyrolysis on granular active carbon aggregate surface forms pyrolytic carbon, strengthens aggregate
Structural strength, improve the conductive capability of activated carbon aggregate；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is being formed by granulated pellet
Other impurity produced during pyrolytic carbon washes, and is placed in vacuum drying oven and is dried 7h after washing, is dried temperature
Degree is 60 DEG C, and vacuum is 100kPa, obtains the carbon for lead carbon battery and is coated with powder composite.
Claims (8)
1. the preparation method for the carbon cladding powder composite of lead carbon battery, it is characterised in that include following step
Rapid:
(1) glucose, sucrose and deionized water are mixed to get mixed liquor A, Hydrocerussitum (Ceruse) is mixed to get with deionized water
Mixed liquid B；Obtain mixed liquor C after mixed liquor A being mixed and stirred for uniformly with B, this mixed liquor C is added hydro-thermal
In reactor, at 160～200 DEG C, disperse 10～12h；
(2) take out the mixed liquor C in hydrothermal reaction kettle, remove the supernatant, obtain colloidal sol D；Utilize and be spray-dried
Machine carries out mist projection granulating to this colloidal sol D；
(3) under inert gas shielding, the granule that step (2) obtains is carried out carbonization so that granular active carbon is reunited
The carbon source pyrolysis of surface forms pyrolytic carbon；
(4) granule obtained step (3) with ethanol and deionized water alternately washs, and is placed in true after washing
Empty drying baker is dried 6～10h, i.e. obtains the described carbon for lead carbon battery and be coated with powder composite.
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levy and be: glucose described in step (1) and the gross weight of sucrose are 1:(4～50 with the weight ratio of deionized water).
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levy and be: Hydrocerussitum (Ceruse) described in step (1) is 1:(2.5～4 with the weight ratio of deionized water).
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levy and be: glucose described in step (1) is (2～12) with the gross weight of sucrose and the weight ratio of Hydrocerussitum (Ceruse): 100.
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levy and be: a diameter of 100～200 μm of mist projection granulating gained granule in step (2).
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levy and be: in step (2), mist projection granulating uses atomizer pelletize, and centrifugal rotational speed is 120～400r/min, temperature
It it is 50～90 DEG C.
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levying and be: in step (3), constant temperature carburizing temperature is 400～600 DEG C, carbonization time is 2～6h.
Carbon for lead carbon battery the most according to claim 1 is coated with the preparation method of powder composite, and it is special
Levying and be: in step (4), baking temperature is 40～60 DEG C, vacuum is 20～100kPa.
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| CN112928261A (en) * | 2021-02-24 | 2021-06-08 | 超威电源集团有限公司 | Lead powder with lead oxide graphene core-shell structure and preparation method thereof |
| CN115286034A (en) * | 2022-07-07 | 2022-11-04 | 中国科学院福建物质结构研究所 | Preparation method of basic lead sulfate material, basic lead sulfate material and application |
| CN115286034B (en) * | 2022-07-07 | 2023-11-17 | 中国科学院福建物质结构研究所 | Preparation method of basic lead sulfate material, basic lead sulfate material and application |
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