CN106480548A - A kind of preparation method of high-specific surface area lead charcoal composite nano fiber - Google Patents
A kind of preparation method of high-specific surface area lead charcoal composite nano fiber Download PDFInfo
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Abstract
The present invention relates to macromolecular material and technical field of chemical power, particularly a kind of preparation method of high-specific surface area lead charcoal composite nano fiber.First pass through electrostatic spinning technique and prepare composite nano fiber, be then passed through noble gases high-temperature calcination and obtain lead charcoal composite nano fiber.Lead particle in-situ is grown in nanofiber surface, lead charcoal binding ability is strong, and has larger specific surface area and compare electric capacity.Preparation process is simple of the present invention, fiber shape can control, and diameter is in Nano grade, low production cost.The lead charcoal composite nano fiber that the present invention provides, solve the problems, such as that in lead carbon battery, material with carbon element easily departs from from active substance, its high specific surface area and restrain oneself ability than what electric capacity can effectively improve the active material utilization of lead carbon battery and high current charge-discharge simultaneously, has broad application prospects in high-performance lead-acid field of batteries.
Description
Technical field
The present invention relates to macromolecular material and technical field of chemical power, particularly a kind of high-specific surface area lead charcoal is again
Close the preparation method of nanofiber.
Background technology
Due to limiting the shortcomings of traditional lead acid batteries specific energy is low, cycle life is short, quick charge capability is poor
It is further applied, the especially application in hybrid vehicle and intermittent energy source storage art, this
Just secondary cell is proposed with partial state of charge state and will have good high current charge-discharge ability and longer circulation longevity
The requirement of life.Lead carbon battery technology, as a kind of emerging lead-acid battery technology, refers to bear in traditional lead acid batteries
The extremely middle material with carbon element adding high-specific surface area, for example：Activated carbon, carbon fiber, carbon aerogels, CNT or
Graphene etc..By the high-specific-power of electric double layer capacitance, long-life blend of predominance in lead-acid battery.Due to height
Specific surface area material with carbon element has the property of high specific capacitance, in moment storage or release electric charge, negative plate is played
Buffer current effect well.Meanwhile, also improve in the high conductivity of high-specific surface area material with carbon element and dispersibility
The utilization rate of active substance, and effectively inhibit growing up and inactivating of sulphuric acid leading crystal in negative plate, extend battery
Cycle life under the conditions of high magnification partial state of charge (HRPSOC).
At present, what lead charcoal negative pole mainly adopted adds material with carbon element or lead button Surface coating material with carbon element in lead negative pole
Method be prepared, but different types of material with carbon element property difference is larger, and Hydrocerussitum (Ceruse) and material proportion differ very
Greatly, it is difficult to realize both uniform mixing, cause the steadiness of lead plaster and adhesion to reduce it is difficult to ensure negative pole
The intensity requirement of plate.Meanwhile, carbon dust is easy to spread in the battery, causes the inefficacy of battery.
Content of the invention
In order to solve ask low with lead plaster adhesion of dispersed difficulty of material with carbon element in existing lead carbon battery negative plate
Topic, it is an object of the invention to provide a kind of preparation method of high-specific surface area lead charcoal composite nano fiber, passes through
Lead particle in-situ is grown in nanofiber surface by electrostatic spinning technique, is then passed through noble gases high-temperature calcination and obtains
To lead charcoal composite nano fiber.
The present invention solves technical problem and adopts the following technical scheme that：
A kind of preparation method of high-specific surface area lead charcoal composite nano fiber, comprises the steps：
1) preparation of spinning liquid：High molecular polymer is added in a certain amount of solvent with certain proportion, water-bath
Under the conditions of stir, obtain spinning liquid；
Wherein, high molecular polymer and the mass ratio of solvent are 5:95 to 20:80, bath temperature is 40～80 DEG C；
2) organic coordination compound of lead is proportionally added into step 1) described in spinning liquid in, by stirring or
Ultrasonic mode makes it be uniformly dispersed, and obtains composite spinning liquid；
Wherein, the organic coordination compound of lead and the mol ratio of high molecular polymer are 1:3～4:1；
3) by step 2) the composite spinning liquid that obtains obtains nanofiber, nanofiber using electrostatic spinning technique
A diameter of 10～500nm；
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding；
Wherein, Pre oxidation is 200～400 DEG C, and temperature retention time is 0.5～4h；Carburizing temperature be 600～
1500 DEG C, temperature retention time is 0.5～10h, and inert protective atmosphere is nitrogen or argon.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 1) in, electrostatic spinning mistake
High molecular polymer in journey is politef, polyacrylonitrile, poly(ethylene oxide) or Polyethylene Glycol.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 1) in, solvent is diformazan
Base Methanamide or dimethyl acetylamide.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 1) in, high molecular polymerization
Thing is 0.5～24h with the mixing time of solvent.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 2) in, the organic of lead joins
Compound is lead acetate, lead citrate, lead oxalate or lead tartrate.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 2) in, the organic of lead joins
Mixing time in spinning liquid for the compound is 1～24h, and ultrasonic time is 0.5～10h.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 3) in, electrostatic spinning work
Skill parameter is：Needle aperture be 0.3～2.0mm, syringe capacity be 5～500mL, spinning flow velocity be 0.2～
5mL/h, the rotating speed of transfer roller is 100～1000r/min, and the voltage between syringe needle and transfer roller is 10～50kV, pin
Head is 10～50cm with the distance between the collecting nanofibers plate on transfer roller, and spinning temperature is 20～50 DEG C,
Spinning humidity is 20～70%RH.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, the collecting nanofibers plate on transfer roller
For one of carbon paper, carbon cloth, graphite paper, aluminium foil, tinfoil paper, alumina foil, carbon paper, graphite paper thickness are
30～300 μm, the thickness of carbon cloth is 100～1000 μm, aluminium foil, tinfoil paper, the thickness of alumina foil is 10～
100μm.
The preparation method of described high-specific surface area lead charcoal composite nano fiber, step 4) in, pre-oxidation treatment
Programming rate be 2～25 DEG C/min, the programming rate of carbonization treatment is 2～25 DEG C/min, inertia shielding gas
Gas flow in atmosphere is 20～100mL/min.
Compared with prior art, advantages of the present invention and beneficial effect are：
1st, the preparation method of the lead charcoal composite nano fiber of the present invention, using electrostatic spinning and subsequent heat treatment,
During this, lead particle in-situ is grown in nanofiber surface, so that lead charcoal binding ability is strengthened, solve biography
The detached shortcoming of lead charcoal that the outer carbon dope source of system lead carbon battery is caused greatly because of the density variation of lead, carbon.
2nd, the preparation method of lead charcoal composite nano fiber of the present invention, used electrospinning device is simple, experiment
Condition is content with very little, and can control the pattern of fiber, composition, knot well by Control release parameter etc.
Structure etc..
3rd, preparation method proposed by the present invention can obtain the lead charcoal composite fibre of Nano grade, and it has larger
Specific surface area and ratio electric capacity, substantially increase suffertibility and the high magnification lotus of the high current charge-discharge of negative material
Cycle life under electric state.
4th, the preparation method of the present invention is cheap, and preparation process is simple is it is easy to operate, favorable repeatability.
5th, the lead charcoal composite nano fiber of the present invention, fiber shape can control, and diameter is in Nano grade.
6th, the lead charcoal composite nano fiber that the present invention provides, solves in lead carbon battery material with carbon element easily from active substance
The problem departing from, its high specific surface area and the active substance profit that lead carbon battery can be effectively improved than electric capacity simultaneously
Restrain oneself ability with rate and high current charge-discharge, have broad application prospects in high-performance lead-acid field of batteries.
Brief description
Fig. 1 is the surface sweeping electron microscopic picture of lead charcoal composite nano fiber.
Specific embodiment
In a specific embodiment, the preparation method of high-specific surface area lead charcoal composite nano fiber of the present invention, first
Composite nano fiber is prepared by electrostatic spinning technique, is then passed through noble gases high-temperature calcination and obtains lead charcoal again
Close nanofiber.Lead particle in-situ is grown in nanofiber surface, lead charcoal binding ability is strong, and has relatively
Big specific surface area and compare electric capacity.Wherein, specific surface area scope is 10～500m2/ g, than capacitance range be 2～
400F/g.Carry out according to following steps and process：
1) preparation of spinning liquid：High molecular polymer is added in a certain amount of solvent with certain proportion, water-bath bar
Stir under part；Wherein, high molecular polymer (politef, polyacrylonitrile, poly(ethylene oxide) or poly-
Ethylene glycol) it is 5 with the mass ratio of solvent (dimethylformamide or dimethyl acetylamide):95 to 20:80 is (excellent
Elect 10 as:90 to 15:85), bath temperature is 40～80 DEG C, and mixing time is high molecular polymer in a solvent
0.5～24h.
2) organic coordination compound (lead acetate, lead citrate, lead oxalate or lead tartrate) of lead is proportionally added into
To step 1) described in spinning liquid in, by stirring or ultrasonic by way of so that it is uniformly dispersed, be combined
Spinning liquid.The organic coordination compound of lead mixing time in spinning liquid is 1～24h (preferably 6～18h), ultrasonic
Time is 0.5～10h (preferably 2～6h).Wherein, the organic coordination compound of the lead being added is high with spinning liquid
The mol ratio of Molecularly Imprinted Polymer is 1:3～4:1 (preferably 1:1～3:1).
3) by step 2) the composite spinning liquid that obtains obtains nanofiber, nanofiber using electrostatic spinning technique
A diameter of 10～500nm (preferably 0.1～10 μm).Wherein, the technological parameter of electrostatic spinning is：Syringe needle hole
Footpath is 0.3～2.0mm, and syringe capacity is 5～500mL, and spinning flow velocity is 0.2～5mL/h, transfer roller
Rotating speed is 100～1000r/min, and the voltage between syringe needle and transfer roller is receiving on 10～50kV, syringe needle and transfer roller
Rice the distance between fiber collecting board is 10～50cm, and spinning temperature is 20～50 DEG C, spinning humidity is 20～
70%RH.Collecting nanofibers plate on transfer roller is carbon paper, carbon cloth, graphite paper, aluminium foil, tinfoil paper, aluminium oxide
One of paper tinsel, carbon paper, graphite paper thickness are 30～300 μm, and the thickness of carbon cloth is 100～1000 μm, aluminum
Paper tinsel, tinfoil paper, the thickness of alumina foil are 10～100 μm.
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding.Wherein, Pre oxidation is 200～400 DEG C, rises
Warm speed is 2～25 DEG C/min, and temperature retention time is 0.5～4h；Carburizing temperature is 600～1500 DEG C, and heat up speed
Spend for 2～25 DEG C/min, temperature retention time is 0.5～10h；Inert protective atmosphere is nitrogen or argon, gas
Flow is 20～100mL/min.
For being best understood from the present invention, with reference to embodiment, the present invention will be further described, but the present invention will
The scope asking protection is not limited to the scope that embodiment represents.
Embodiment 1
1) mass fraction is that 10% polyacrylonitrile is added in dimethylformamide under agitation, water-bath
At temperature is 60 DEG C, stirring 2h obtains spinning liquid, and the mean molecule quantity of polyacrylonitrile is 150000.
2) lead acetate is added in spinning liquid, added lead acetate with the mol ratio of polyacrylonitrile in spinning liquid is
3:1, after stirring 12h, more ultrasonic 6h, obtain uniform composite spinning liquid.
3) by through step 2) the composite spinning liquid that obtains is added in the syringe of 5mL, using Static Spinning
Silk technology obtains nanofiber, and nanofiber diameter is 2 μm.Wherein, the technological parameter of electrostatic spinning is：Pin
Head bore footpath is 1mm, and syringe capacity is 100mL, and spinning flow velocity is 0.5mL/h, and the rotating speed of transfer roller is
300r/min, the voltage between syringe needle and transfer roller is 25kV, between the collecting nanofibers plate on syringe needle and transfer roller
Distance be 20cm, spinning temperature be 30 DEG C, spinning humidity be 40%RH.The collection of nanofiber on transfer roller
Plate is carbon paper, and thickness is 100 μm.
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding.Wherein, Pre oxidation is 300 DEG C, and heat up speed
Spend for 5 DEG C/min, temperature retention time is 3h；Carburizing temperature is 1000 DEG C, and programming rate is 5 DEG C/min, insulation
Time is 6h；Inert protective atmosphere is nitrogen or argon, and gas flow is 50mL/min.
As shown in figure 1, the surface sweeping electron microscopic picture of lead charcoal composite nano fiber.In the present embodiment, using Static Spinning
With respect to traditional lead carbon composite, specific surface area greatly improves the lead charcoal composite nano fiber that silk technology is prepared,
Lead charcoal adhesion is remarkably reinforced, and high current charge-discharge suffertibility is substantially improved.Wherein, specific surface area scope is
100～150m2/ g, is 50～60F/g than capacitance range..
Embodiment 2
1) mass fraction is that 15% politef is added in dimethylformamide under agitation, water
At bath temperature is 60 DEG C, stirring 2h obtains spinning liquid, and the mean molecule quantity of politef is 13000.
2) lead citrate is added in spinning liquid, added lead citrate and the rubbing of politef in spinning liquid
That ratio is 1:1, after stirring 15h, more ultrasonic 4h, obtain uniform composite spinning liquid.
3) by through step 2) the composite spinning liquid that obtains is added in the syringe of 10mL, using Static Spinning
Silk technology obtains nanofiber, and nanofiber diameter is 1 μm.Wherein, the technological parameter of electrostatic spinning is：Pin
Head bore footpath is 1.5mm, and syringe capacity is 50mL, and spinning flow velocity is 1mL/h, and the rotating speed of transfer roller is
200r/min, the voltage between syringe needle and transfer roller is 20kV, between the collecting nanofibers plate on syringe needle and transfer roller
Distance be 30cm, spinning temperature be 40 DEG C, spinning humidity be 30%RH.The collection of nanofiber on transfer roller
Plate is alumina foil, and thickness is 50 μm.
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding.Wherein, Pre oxidation is 200 DEG C, and heat up speed
Spend for 3 DEG C/min, temperature retention time is 4h；Carburizing temperature is 1500 DEG C, and programming rate is 15 DEG C/min, insulation
Time is 2h；Inert protective atmosphere is nitrogen or argon, and gas flow is 60mL/min.
As shown in figure 1, the surface sweeping electron microscopic picture of lead charcoal composite nano fiber.In the present embodiment, using Static Spinning
With respect to traditional lead carbon composite, specific surface area greatly improves the lead charcoal composite nano fiber that silk technology is prepared,
Lead charcoal adhesion is remarkably reinforced, and high current charge-discharge suffertibility is substantially improved.Wherein, specific surface area scope is
120～150m2/ g, is 70～90/g than capacitance range..
Embodiment 3
1) mass fraction is that 12% poly(ethylene oxide) is added in dimethylformamide under agitation, water
At bath temperature is 60 DEG C, stirring 2h obtains spinning liquid, and the mean molecule quantity of poly(ethylene oxide) is 12000.
2) lead oxalate is added in spinning liquid, the mol ratio of poly(ethylene oxide) in added lead oxalate and spinning liquid
For 2:1, after stirring 8h, more ultrasonic 8h, obtain uniform composite spinning liquid.
3) by through step 2) the composite spinning liquid that obtains is added in the syringe of 15mL, using Static Spinning
Silk technology obtains nanofiber, and nanofiber diameter is 3 μm.Wherein, the technological parameter of electrostatic spinning is：Pin
Head bore footpath is 2mm, and syringe capacity is 150mL, and spinning flow velocity is 1.5mL/h, and the rotating speed of transfer roller is
400r/min, the voltage between syringe needle and transfer roller is 30kV, between the collecting nanofibers plate on syringe needle and transfer roller
Distance be 10cm, spinning temperature be 50 DEG C, spinning humidity be 50%RH.The collection of nanofiber on transfer roller
Plate is tinfoil paper, and thickness is 30 μm.
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding.Wherein, Pre oxidation is 400 DEG C, and heat up speed
Spend for 15 DEG C/min, temperature retention time is 1h；Carburizing temperature is 1200 DEG C, and programming rate is 10 DEG C/min, protects
The warm time is 5h；Inert protective atmosphere is nitrogen or argon, and gas flow is 80mL/min.
As shown in figure 1, the surface sweeping electron microscopic picture of lead charcoal composite nano fiber.In the present embodiment, using Static Spinning
With respect to traditional lead carbon composite, specific surface area greatly improves the lead charcoal composite nano fiber that silk technology is prepared,
Lead charcoal adhesion is remarkably reinforced, and high current charge-discharge suffertibility is substantially improved.Wherein, specific surface area scope is
140～180m2/ g, is 180～200F/g than capacitance range..
Embodiment 4
1) mass fraction is that 13% Polyethylene Glycol is added in dimethylformamide under agitation, water-bath
At temperature is 60 DEG C, stirring 2h obtains spinning liquid, and the mean molecule quantity of Polyethylene Glycol is 8000.
2) lead tartrate is added in spinning liquid, in added lead tartrate and spinning liquid Polyethylene Glycol mole
Than for 2.5:1, after stirring 16h, more ultrasonic 3h, obtain uniform composite spinning liquid.
3) by through step 2) the composite spinning liquid that obtains is added in the syringe of 20mL, using Static Spinning
Silk technology obtains nanofiber, and nanofiber diameter is 0.5 μm.Wherein, the technological parameter of electrostatic spinning is：
Needle aperture is 0.5mm, and syringe capacity is 200mL, and spinning flow velocity is 3mL/h, and the rotating speed of transfer roller is
500r/min, the voltage between syringe needle and transfer roller is 45kV, between the collecting nanofibers plate on syringe needle and transfer roller
Distance be 40cm, spinning temperature be 20 DEG C, spinning humidity be 60%RH.The collection of nanofiber on transfer roller
Plate is graphite paper, and thickness is 60 μm.
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding.Wherein, Pre oxidation is 350 DEG C, and heat up speed
Spend for 10 DEG C/min, temperature retention time is 2h；Carburizing temperature is 800 DEG C, and programming rate is 3 DEG C/min, insulation
Time is 8h；Inert protective atmosphere is nitrogen or argon, and gas flow is 30mL/min.
As shown in figure 1, the surface sweeping electron microscopic picture of lead charcoal composite nano fiber.In the present embodiment, using Static Spinning
With respect to traditional lead carbon composite, specific surface area greatly improves the lead charcoal composite nano fiber that silk technology is prepared,
Lead charcoal adhesion is remarkably reinforced, and high current charge-discharge suffertibility is substantially improved.Wherein, specific surface area scope is
100～130m2/ g, is 50～70F/g than capacitance range..
Claims (9)
1. a kind of preparation method of high-specific surface area lead charcoal composite nano fiber is it is characterised in that include following walking
Suddenly：
1) preparation of spinning liquid：High molecular polymer is added in a certain amount of solvent with certain proportion, water-bath
Under the conditions of stir, obtain spinning liquid；
Wherein, high molecular polymer and the mass ratio of solvent are 5:95 to 20:80, bath temperature is 40～80 DEG C；
2) organic coordination compound of lead is proportionally added into step 1) described in spinning liquid in, by stirring or
Ultrasonic mode makes it be uniformly dispersed, and obtains composite spinning liquid；
Wherein, the organic coordination compound of lead and the mol ratio of high molecular polymer are 1:3～4:1；
3) by step 2) the composite spinning liquid that obtains obtains nanofiber, nanofiber using electrostatic spinning technique
A diameter of 10～500nm；
4) by step 3) nanofiber that obtains pre-oxidized and carbonization through atmosphere furnace, cools to room with the furnace
Temperature, can get lead charcoal composite nano fiber through grinding；
Wherein, Pre oxidation is 200～400 DEG C, and temperature retention time is 0.5～4h；Carburizing temperature be 600～
1500 DEG C, temperature retention time is 0.5～10h, and inert protective atmosphere is nitrogen or argon.
2. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 1) in, the high molecular polymer during electrostatic spinning is politef, polyacrylonitrile,
Poly(ethylene oxide) or Polyethylene Glycol.
3. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 1) in, solvent is dimethylformamide or dimethyl acetylamide.
4. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 1) in, high molecular polymer is 0.5～24h with the mixing time of solvent.
5. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 2) in, the organic coordination compound of lead is lead acetate, lead citrate, lead oxalate or lead tartrate.
6. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 2) in, the organic coordination compound of the lead mixing time in spinning liquid is 1～24h, when ultrasonic
Between be 0.5～10h.
7. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 3) in, electrostatic spinning process parameter is：Needle aperture is 0.3～2.0mm, and syringe holds
Measure as 5～500mL, spinning flow velocity is 0.2～5mL/h, the rotating speed of transfer roller is 100～1000r/min, pin
Voltage between head and transfer roller is that the distance between collecting nanofibers plate on 10～50kV, syringe needle and transfer roller is
10～50cm, spinning temperature is 20～50 DEG C, and spinning humidity is 20～70%RH.
8. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 7, it is special
Levy and be, the collecting nanofibers plate on transfer roller is carbon paper, carbon cloth, graphite paper, aluminium foil, tinfoil paper, aluminium oxide
One of paper tinsel, carbon paper, graphite paper thickness are 30～300 μm, and the thickness of carbon cloth is 100～1000 μm, aluminum
Paper tinsel, tinfoil paper, the thickness of alumina foil are 10～100 μm.
9. the preparation method of high-specific surface area lead charcoal composite nano fiber according to claim 1, it is special
Levy and be, step 4) in, the programming rate of pre-oxidation treatment is 2～25 DEG C/min, the intensification of carbonization treatment
Speed is 2～25 DEG C/min, and the gas flow in inert protective atmosphere is 20～100mL/min.
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| CN110541210A (en) * | 2019-09-04 | 2019-12-06 | 中国科学院宁波材料技术与工程研究所 | Nitrogen-rich porous polyacrylonitrile-based carbon fiber and preparation method and application thereof |
| CN110541210B (en) * | 2019-09-04 | 2021-12-21 | 中国科学院宁波材料技术与工程研究所 | Nitrogen-rich porous polyacrylonitrile-based carbon fiber and preparation method and application thereof |
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