CN106654306B - A kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst - Google Patents
A kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst Download PDFInfo
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- CN106654306B CN106654306B CN201611053657.XA CN201611053657A CN106654306B CN 106654306 B CN106654306 B CN 106654306B CN 201611053657 A CN201611053657 A CN 201611053657A CN 106654306 B CN106654306 B CN 106654306B
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst, operating procedure: (1) being dismantled useless lithium thionyl chloride cell, collects sulphur/carbon black mixt after discharging in battery；(2) it keeps temperature to be 500~1100 DEG C in inert gas and carries out heat treatment 10~150 minutes, it is cooling；(3) it is added in acid solution and stirs 2~10 hours, then filter, wash with water filter residue to efflux and be in neutrality, filter residue and drying to moisture is less than 5wt%, collects to obtain the final product.The method of the present invention obtains sulfur doping carbon oxygen reduction electro-catalyst, and the catalyst effect is good, and preparation method is simple, is easy to produce in batches；The present invention is that while substantially reducing production cost, also effectively solve the problems, such as discarded lithium Asia battery difficulty recycling by recycling the waste, pollute the environment；The method of the present invention is simple and easy, economic and environment-friendly, is easy to scale, has broad application prospects, economic benefit value and social enviroment protection are worth.
Description
Technical field
The present invention relates to a kind of preparation method of elctro-catalyst, in particular to a kind of sulfur doping carbon oxygen reduction electro-catalyst
Preparation method.
Background technique
Fuel cell has many advantages, such as environmental-friendly, and running temperature is low and high-energy source conversion ratio, it is considered to be the end of the mankind
The pole energy [Chem.Rev.2004,104,4245；New material industry, 2015,4,58].However the mistake that Cathodic oxygen reduction is high
Current potential and slow kinetics restrict the large-scale commercial application of fuel cell.Platinum catalyst is hydrogen reduction best at present
Catalysts, but platinum catalyst poisons and [J.Power the disadvantages of platinum scarcity of resources vulnerable to carbon monoxide there are expensive
Sources,2006,156,171；Electrochim.Acta,2011,56,9186].Develop inexpensive non-precious metal catalyst
Substitution platinum catalyst be large-scale commercial application fuel cell there is an urgent need to.Heteroatom doping carbon material is adjustable carbon material
Structure, characteristic electron and physicochemical properties, hydrogen reduction overpotential or even some doping carbon materials, which is effectively reduced, to be had and platinum
Catalyst is suitable or more superior hydrogen reduction electro catalytic activity, and has high stability and good anti-carbon monoxide
[Science.2009,323,760；Nano Energy,2016,19,373].
Sulphur atom adulterates carbon material, adjusts sp in carbon material by lone pair electrons on sulphur atom2The Π electron of hydridization carbon
System, can effectively improve its hydrogen reduction performance [Electrochemistry Communications.2013,30,9；
J.Mater.Chem.A,2016,4,83].However, sulfur doping carbon materials preparation method for material has equipment requirement height (if you need to cold at present
Dry or supercritical drying device [a kind of preparation method of sulfur doping carbon material, CN104860296A] is lyophilized), the reaction time it is long,
Raw material it is extremely toxic (such as trithiocyanuric acid [a kind of preparation method of the nitride porous carbon catalysis material of sulfur doping,
CN103861632A]), reaction step cumbersome [a method of efficiently prepare sulfur doping hollow carbon sphere, CN105293468A], produce
Measure it is low, expensive [a kind of doping of nitrogen phosphate and sulfur or codope carbon dots and its batch controllable method for preparing and application,
CN104987863A] the disadvantages of, it is unfavorable for the inexpensive mass preparation of sulfur doping carbon material.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
Present invention seek to address that currently useless lithium thionyl chloride cell recycling difficult problem and sulfur doping carbon consuming cell is non-
Equipment requirement present in noble metal sulfur doping carbon oxygen reduction electro-catalyst preparation process is high, the reaction time is long, raw material is extremely toxic, anti-
Answer complex steps, low output, it is expensive the problems such as, invent a kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst, benefit
Sulfur doping carbon oxygen reduction catalyst is prepared with the lithium thionyl chloride cell that gives up after electric discharge, has simple and easy, can be mass, it is economical
The advantage of environmental protection.
To achieve the above object, technical solution provided by the invention is as follows:
A kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst includes following operating procedure:
(1) useless lithium thionyl chloride cell is dismantled, collects sulphur/carbon black mixt after discharging in battery；
(2) gained sulphur/carbon black mixt in step (1) is kept temperature in inert gas is 500~1100 DEG C of progress
Heat treatment 10~150 minutes, it is cooling；
(3) will it is cooling in step (2) after gained sulphur/carbon black mixt be added in acid solution and stir 2~10 hours, then mistake
Filter, washes with water filter residue to efflux and is in neutrality, and filter residue and drying to moisture is less than 5wt%, collects to obtain the final product, as sulfur doping carbon oxygen
Restore elctro-catalyst.
Preferably, indifferent gas described in step (2) is a kind of in nitrogen, argon gas or hydrogen.
Preferably, heat treatment temperature described in step (2) is 700~900 DEG C.
Preferably, heat treatment time described in step (2) is 30~60 minutes.
Preferably, the acid solution of 10~1000ml is added in step (3) to gained sulphur/carbon black mixt 1g after cooling.
Preferably, acid solution described in step (3) is in sulfuric acid solution, hydrochloric acid solution, nitric acid solution or hydrofluoric acid
One or more kinds of mixtures.
Preferably, acid solutions described in step (3) are 1~5mol/L.
Preferably, mixing time described in step (3) is 4~8 hours.
Sulfur doping carbon oxygen reduction electro-catalyst obtained by above-mentioned preparation is used as the elctro-catalyst of fuel cell.
Compared with prior art, the invention has the following beneficial effects:
The method of the present invention obtains sulfur doping carbon oxygen reduction electro-catalyst, and the catalyst effect is good, and preparation method letter
It is single, it is easy to produce in batches；The present invention is that while substantially reducing production cost, also effectively solve by recycling the waste
The problem of discarded lithium Asia battery difficulty is recycled, is polluted the environment；The method of the present invention is simple and easy, economic and environment-friendly, is easy to scale
Change, has broad application prospects, economic benefit value and social enviroment protection are worth.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the preparation of implementation column 1 gained sulfur doping carbon oxygen reduction electro-catalyst of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of the preparation gained sulfur doping carbon oxygen reduction electro-catalyst of the embodiment of the present invention 1.
Fig. 3 is that the preparation gained sulfur doping carbon oxygen reduction electro-catalyst of the embodiment of the present invention 1 makes as oxygen reduction electro-catalyst
The linear scan curve of used time.
Fig. 4 is that the preparation gained sulfur doping carbon oxygen reduction electro-catalyst of the embodiment of the present invention 1 makes as oxygen reduction electro-catalyst
Constant potential (when m- electric current) curve of used time.
Specific embodiment
Specific embodiment is described in detail with reference to the accompanying drawing, it is to be understood that protection scope of the present invention not by
The limitation of specific embodiment.
Embodiment 1
A kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst, operating procedure are as follows:
(1) useless lithium thionyl chloride cell (ER14250) is dismantled, collects sulphur/carbon black mixt after discharging in battery；
(2) it keeps temperature to be 800 DEG C in nitrogen gained sulphur/carbon black mixt in step (1) and carries out 30 points of heat treatment
Clock, it is cooling；
(3) it is 1mol/L hydrochloric acid solution that 100ml concentration, which is added, in gained sulphur/carbon black mixt 1g after will be cooling in step (2)
Middle stirring 6 hours, then filters, takes filter residue to be washed with deionized water to the deionized water of outflow and be in neutrality, dry filter residue to moisture
Less than 5wt%, collect up to sample, as sulfur doping carbon oxygen reduction electro-catalyst.
Embodiment 2
A kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst, operating procedure are as follows:
(1) useless lithium thionyl chloride cell (ER14250) is dismantled, collects sulphur/carbon black mixt after discharging in battery；
(2) it keeps temperature to be 500 DEG C in nitrogen gained sulphur/carbon black mixt in step (1) and carries out 150 points of heat treatment
Clock, it is cooling；
(3) will it is cooling in step (2) after gained concentration is added is to stir 2 hours in 5mol/L10ml sulfuric acid solution, then
Filtering, cleans filter residue to efflux with deionized water and is in neutrality, and gained filter residue and drying to moisture is less than 5wt%, collects up to sulphur
Doped carbon oxygen reduction electro-catalyst.
Embodiment 3
A kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst, operating procedure are as follows:
(1) useless lithium thionyl chloride cell (ER14250) is dismantled, collects sulphur/carbon black mixt after discharging in battery；
(2) it keeps temperature to be 1100 DEG C in hydrogen gained sulphur/carbon black mixt in step (1) and carries out 10 points of heat treatment
Clock, it is cooling；
(3) will it is cooling in step (2) after gained nitric acid solution that concentration is 3mol/L1000ml is added and hydrofluoric acid mixes
Stirring 10 hours in acid solution (nitric acid solution and 3mol/L hydrofluoric acid solution volume ratio 1:1 of 3mol/L mixes), then filter,
It cleans filter residue to efflux with deionized water to be in neutrality, gained filter residue and drying to moisture is less than 5wt%, collects up to sulfur doping carbon
Oxygen reduction electro-catalyst.
Gained sample is prepared with the embodiment of the present invention 1 and carries out X-ray diffraction, scanning electron microscope, as shown in Fig. 1~2；Gained sample
Product do X-ray photoelectron spectroscopic analysis, and the data obtained is as shown in table 1:
Table 1
| Element | Peak position eV | Peak height CPS | Atomic ratio % |
| C1s | 284.81 | 16487.95 | 85.7 |
| O1s | 532.28 | 1612.21 | 8.62 |
| S2p | 163.73 | 1059.14 | 5.68 |
Sulfur doping carbon oxygen reduction electro-catalyst is shown sharp apparent in 2 θ=26.3 ° it can be seen from Fig. 1 and table 1
Graphite peaks, surface sulfur content account for total atom 5.68%；
The micro-raman spectra of sample as seen from Figure 2, sulfur doping carbon oxygen reduction electro-catalyst show the canonical form of carbon black
Looks；
Fig. 3 is that sulfur doping carbon reduction elctro-catalyst 5mV/s in the 0.1mol/L potassium hydroxide solution that oxygen is saturated sweeps speed
Under the conditions of linear scan curve, the hydrogen reduction of sulfur doping carbon oxygen reduction electro-catalyst plays spike potential and reaches 0.97V in figure, very
Business platinum carbon (Pt/C) catalyst close to current hydrogen reduction optimum activity plays spike potential (1.0V vs.RHE)；Sulfur doping simultaneously
Carbon illustrates apparent hydrogen reduction carrying current platform, and hydrogen reduction carrying current is 5.3mA/cm2, it is slightly larger than (being better than) quotient
The carrying current of industry Pt/C；
Constant potential (when m- electric current) curve that Fig. 4 is sulfur doping carbon oxygen reduction electro-catalyst as oxygen reduction catalyst, sulphur
Doped carbon oxygen reduction electro-catalyst has the stability for being substantially better than business platinum carbon catalyst, only has after 3h potentiostatic scanning
4.6% current loss, and business platinum carbon catalyst has 31.2% current loss.
To sum up, great practical application value in terms of sulfur doping carbon oxygen reduction electro-catalyst prepared by the present invention.
Inventor has found in lithium thionyl chloride cell unintentionally in the course of the research, due to the thionyl chloride (sulfurous of liquid phase
Acyl chlorides) it is contacted with carbon black with good, in-situ reducing generates sulphur simple substance and is carried on carbon black in discharge process, has highly uniform
Dispersibility and strong mutual active force, carbon black can conductive well and buffering inhibit sulphur volume expansion, thus have good
Lithium-sulfur electrochemical performance.Lithium thionyl chloride cell is widely used, and only Chinese annual lithium thionyl chloride cell consumption is more than one hundred million
Only, the method prepares Lithium-sulphur battery anode material using discarded lithium thionyl chloride cell recycling, simple and easy, economic and environment-friendly,
It is easy to scale, has broad application prospects, economic benefit value and social enviroment protection are worth.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (9)
1. a kind of preparation method of sulfur doping carbon oxygen reduction electro-catalyst, which is characterized in that include following operating procedure:
(1) useless lithium thionyl chloride cell is dismantled, collects sulphur/carbon black mixt after discharging in battery；
(2) it keeps temperature to be 500 ~ 1100 DEG C in inert gas gained sulphur/carbon black mixt in step (1) and carries out hot place
Reason 10 ~ 150 minutes, it is cooling；
(3) gained sulphur/carbon black mixt is added in acid solution and stirs 2 ~ 10 hours after will be cooling in step (2), then filters, uses
Water cleaning filter residue to efflux is in neutrality, and filter residue and drying to moisture is collected to obtain the final product less than 5 wt%, as the hydrogen reduction of sulfur doping carbon
Elctro-catalyst.
2. preparation method according to claim 1, it is characterised in that: inert gas described in step (2) is nitrogen, argon
It is a kind of in gas or hydrogen.
3. preparation method according to claim 1, it is characterised in that: the temperature of heat treatment described in step (2) be 700 ~
900 ℃。
4. preparation method according to claim 1, it is characterised in that: the time of heat treatment described in step (2) is 30 ~ 60
Minute.
5. preparation method according to claim 1, it is characterised in that: to gained sulphur after cooling/carbon black mixing in step (3)
The acid solution of 10 ~ 1000 ml is added in 1 g of object.
6. preparation method according to claim 1, it is characterised in that: acid solution described in step (3) be sulfuric acid solution,
One of hydrochloric acid solution, nitric acid solution or hydrofluoric acid or more than one mixtures.
7. preparation method according to claim 1, it is characterised in that: the concentration of acid solution described in step (3) is 1 ~ 5
mol/L。
8. preparation method according to claim 1, it is characterised in that: the time of stirring described in step (3) is 4 ~ 8 small
When.
9. preparation method according to claim 1, it is characterised in that: gained sulfur doping carbon oxygen reduction electro-catalyst can be used for
Elctro-catalyst as fuel cell.
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| CN104600247A (en) * | 2014-12-31 | 2015-05-06 | 山东玉皇新能源科技有限公司 | Sulfur-carbon composite positive electrode material for lithium-sulfur battery and preparation method of sulfur-carbon composite positive electrode material |
| CN105552468A (en) * | 2016-01-21 | 2016-05-04 | 河南环宇赛尔新能源科技有限公司 | Recycling method for graphite anode material from waste lithium-ion battery |
| CN105932351A (en) * | 2016-05-16 | 2016-09-07 | 上海赛特康新能源科技股份有限公司 | Resource recycling method for waste lithium batteries |
| CN106058349A (en) * | 2015-04-07 | 2016-10-26 | 罗伯特·博世有限公司 | Utilization of lithium battery |
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| CN104600247A (en) * | 2014-12-31 | 2015-05-06 | 山东玉皇新能源科技有限公司 | Sulfur-carbon composite positive electrode material for lithium-sulfur battery and preparation method of sulfur-carbon composite positive electrode material |
| CN106058349A (en) * | 2015-04-07 | 2016-10-26 | 罗伯特·博世有限公司 | Utilization of lithium battery |
| CN105552468A (en) * | 2016-01-21 | 2016-05-04 | 河南环宇赛尔新能源科技有限公司 | Recycling method for graphite anode material from waste lithium-ion battery |
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