CN110155982A - A kind of carbon burns SBA-15 mesopore molecular sieve and preparation method thereof and its application in water system battery - Google Patents

A kind of carbon burns SBA-15 mesopore molecular sieve and preparation method thereof and its application in water system battery Download PDF

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Publication number
CN110155982A
CN110155982A CN201910436494.0A CN201910436494A CN110155982A CN 110155982 A CN110155982 A CN 110155982A CN 201910436494 A CN201910436494 A CN 201910436494A CN 110155982 A CN110155982 A CN 110155982A
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sba
molecular sieve
mesopore molecular
carbon
burns
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张宏宇
白雪
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Fujian University of Technology
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Fujian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • 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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of carbon to burn SBA-15 mesopore molecular sieve and preparation method thereof and its application in water system battery, it is that the concentrated sulfuric acid and sucrose is soluble in water, and SBA-15 is added and is uniformly mixed, it is dried after filtering repeatedly, then finally obtains the carbon through carbonization treatment for several times and calcining, hydrofluoric acid dips and burn SBA-15 mesopore molecular sieve.Gained carbon burns SBA-15 mesopore molecular sieve and combines the stability of carbon material and the frame of SBA-15 cellular structure, so that water system can deintercalation, adion stablize transmission, it is effectively improved bulk effect, improve cycle performance, it is suitable as the negative electrode material of water system lithium, sodium, Magnesium ion battery, and its abundant raw materials, it is low in cost, it is ideal water system cell negative electrode material.

Description

A kind of carbon burn SBA-15 mesopore molecular sieve and preparation method thereof and its in water system battery Application
Technical field
The invention belongs to electrode material preparation fields, are related to a kind of synthetic method of water system cell negative electrode material, specifically It is that burn SBA-15 mesoporous for the water system battery negative material carbon of achievable water system lithium, sodium, magnesium ion deintercalation or adsorption desorption a kind of that ground, which is said, The preparation method of molecular sieve.
Background technique
With the continuous deterioration of energy crisis and environmental pollution, accelerate the utilization of renewable energy and the construction of smart grid It is the important directions of human kind sustainable development.Energy stores are constantly subjected to the extensive concern of people, wherein battery is as electrochemistry One of energy storage technology, it is closely bound up and inseparable with our life, such as: it is battery of mobile phone, cells in notebook computer, electronic Vehicle tesla battery etc..According to the development course of battery, lead-acid battery is earliest commercialized battery, energy density is low, Cycle life is short；Lithium ion battery is widely used among various industries with its high-energy density, but its organic electrolyte is easy Explosive, pollution environment is fired, and lithium resource is expensive, resource is limited, is not the first choice of human kind sustainable development.Water system battery Be exactly using inorganic salt solution as electrolyte, cooperation can deintercalation positive and negative pole material realize energy storage.Currently, water system electricity applicatory Pond positive electrode has spinel-type LiMn2O4, stratiform LiCoO2, olivine-type LiFePO4And LiMnPO4, it is Prussian blue FeHCF, CuHCF etc.；However it is extremely limited to the research of water system battery negative electrode material applicatory, this is because voltage compared with Electrode material is extremely easy in decomposition in aqueous electrolyte and is often accompanied by the generation of side reaction when low, and only several negative electrode materials are restricted In the short disadvantage of cycle life, it is difficult to realize the application of full battery.
The carbon that the present invention develops, which burns SBA-15 mesopore molecular sieve as water system cell negative electrode material, can realize lithium ion Deintercalation, sodium ion and magnesium ion adsorption-desorption, and be assembled into water system full battery or water system capacitor batteries can express it is excellent Cycle performance is ideal water system cell negative electrode material.At the same time, the present invention selects low-cost raw material, green ring The water system battery system of guarantor is research object, meets the present age to the growth requirement of " second generation energy-storage battery ".
Summary of the invention
It is low in cost the purpose of the present invention is to provide a kind of abundant raw materials, water system battery cathode can be widely used as The carbon of material burns SBA-15 mesopore molecular sieve and its synthetic method, is to carry out filling out carbon calcining as presoma using SBA-15, obtains A kind of carbon material with SBA-15 skeleton mesopore size, cellular structure.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of carbon burning SBA-15 mesopore molecular sieve, preparation method includes the following steps:
1) concentrated sulfuric acid, sucrose is soluble in water, SBA-15 mesopore molecular sieve is added and is sufficiently mixed, 30min is stirred at room temperature, must mix Liquid；
2) gained mixed liquor is filtered, and is washed with filtrate, filtered 5 ~ 10 times repeatedly, gained filter cake is in 70 DEG C of freeze-day with constant temperature Dry 10h in case；
3) obtained solid powder after drying is put into thermostatic drying chamber and is tentatively carbonized, then ground；
4) with preliminary carbonization and polished black powder alternative steps 1) in SBA-15 mesopore molecular sieve, repeat step 1) ~ 3) 2 times；
5) final gained black powder is calcined under nitrogen protection；
6) calcined black powder is impregnated in hydrofluoric acid solution, to remove template, is washed with water and washs to neutrality to get institute It states carbon and burns SBA-15 mesopore molecular sieve.
Concentrated sulfuric acid content is 0.06 ~ 0.11 g/L, cane sugar content 80g/L, SBA-15 Jie in mixed liquor obtained by step 1) Porous molecular sieve content is 53 ~ 100 g/L.Preferably, the content of the concentrated sulfuric acid, sucrose and SBA-15 mesopore molecular sieve is respectively 0.0615g/L, 80g/L, 53.3g/L or 0.082g/L, 80g/L, 66.7g/L or 0.1025g/L, 80g/L, 100g/L.
The temperature being tentatively carbonized described in step 3) is 150 DEG C ~ 180 DEG C, the time is 5h ~ 8h.
The temperature of calcining described in step 5) is 550 DEG C ~ 750 DEG C, the time is 1h ~ 3h.
The mass fraction of hydrofluoric acid solution used in step 6) is 10% ~ 30%, and soaking time is 10h ~ 30h.
Gained carbon of the invention burns the stability of SBA-15 mesopore molecular sieve combination carbon material and the frame of SBA-15 cellular structure Frame so that water system can deintercalation, adion stablize transmission, be effectively improved bulk effect, improve cycle performance, be suitable as water system Cell negative electrode material.Its concrete application method are as follows: SBA-15 mesopore molecular sieve is burnt as active material using carbon, Kynoar is viscous Agent is tied, acetylene black and Ketjen black are conductive agent, and 80%:10%:5%:5% forms slurry by mass percentage by it, by gained Slurry is coated on carbon cloth collector, is dried in vacuo at 75 DEG C and cathode is made, to have reported commercialization material such as LiMn2O4、 Na0.44MnO2Or MnO2Deng be anode, LiNO3、NaNO3Or Mg (NO3)2Aqueous solution be electrolyte assembling be made water system full battery or Capacitor batteries.
The present invention has the advantages that
(1) present invention prepares the burning molecular sieve of the carbon based on SBA-15 meso-hole structure, this nanometer by the method for repeating to fill out carbon Grade carbon material inherits the meso-hole structure of SBA-15, can not only increase the wellability between electrode and electrolyte, be conducive to from The transmission of son and electronics, and there is the mesoporous frame structure of SBA-15, it can be effectively improved bulk effect, improve cyclical stability
(2) pass through electro-chemical test, negative electrode material made from SBA-15 mesopore molecular sieve is burnt in 50 mA g as carbon of the present invention-1Electricity Under current density, 0.5 mol dm−3 Mg(NO3)2In electrolyte, specific capacity is 70.6 mAh g-1；Assemble them into water system capacitor Battery, in 100 mA g-1Under current density, 0.5 mol dm−3 Mg(NO3)2Its capacity is recycled through 800 circles in electrolyte to keep Rate is up to 98.6%, and coulombic efficiency is close to 100%.
(3) carbon prepared by the present invention burns SBA-15 mesopore molecular sieve suitable for water system lithium, sodium, a variety of bodies of magnesium ion System, can be assembled into water system full battery or water system capacitor batteries, can effectively improve water system cycle performance of battery.
Detailed description of the invention
Fig. 1 is the XRD diagram that carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve.
Fig. 2 is SEM (a) and TEM (b) shape appearance figure that carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve.
Fig. 3 is the SEM shape appearance figure that carbon prepared by embodiment 2 burns SBA-15 mesopore molecular sieve.
Fig. 4 is that carbon prepared by embodiment 3 burns SBA-15 mesopore molecular sieve TEM shape appearance figure.
Fig. 5 is that carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve in Mg (NO3)2In electrolyte, 100 mAg-1Electric current Cycle efficieny figure under density；
Fig. 6 is that carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve in Mg (NO3)2In electrolyte, under different current densities High rate performance figure；
Fig. 7 is that the water system magnesium ion capacitor electricity that SBA-15 mesopore molecular sieve is cathode assembling is burnt using carbon prepared by embodiment 1 The cycle efficieny figure in pond.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
1) concentrated sulfuric acid and sucrose are dissolved in 15mL water, SBA-15 mesopore molecular sieve is added and is sufficiently mixed, 30min is stirred at room temperature extremely It is uniformly dispersed, obtains mixed liquor, wherein concentrated sulfuric acid content is 0.082g/L, cane sugar content 80g/L, SBA-15 mesopore molecular sieve contains Amount is 66.7g/L；
2) gained mixed liquor is filtered, and is washed with filtrate, filtered 6 times repeatedly, so that being sufficiently submerged in containing sucrose solution Carbon amounts is filled out with control in SBA-15 mesopore molecular sieve, gained filter cake is then placed in 70 DEG C of thermostatic drying chambers dry 10h, control The coking extent of sucrose；
3) obtained solid powder after drying is put into 160 DEG C of preliminary carbonization 6h in thermostatic drying chamber, is then ground；
4) with preliminary carbonization and polished black powder alternative steps 1) in SBA-15 mesopore molecular sieve, repeat step 1) ~ 3) 2 times；
5) by final gained black powder under nitrogen protection, 700 DEG C of calcining 1.5h；
6) calcined black powder is placed in the hydrofluoric acid solution that mass fraction is 15% and impregnates 30h, to remove template, then It is washed with water to neutrality, obtains target product.
Carbon prepared by the respectively the present embodiment of Fig. 1,2 burns the X powder diffraction figure and electron microscope of SBA-15 mesopore molecular sieve.From It can be seen that its meso pore characteristics peak and cellular structure are obvious in figure.
Embodiment 2
Concentrated sulfuric acid content is 0.0615g/L in gained mixed liquor in 1 step 1) of embodiment, cane sugar content 80g/L, SBA-15 are situated between Porous molecular sieve content is 53.3g/L.Remaining synthesis condition is constant.
The SEM shape appearance figure of the burning SBA-15 mesopore molecular sieve of carbon prepared by Fig. 3 the present embodiment.It can be seen that its reunite compared with It is obvious.
Embodiment 3
It is changed to number is filtered in 1 step 2) of embodiment 8 times.Remaining synthesis condition is constant.
Fig. 4 is the TEM shape appearance figure that carbon prepared by the present embodiment burns SBA-15 mesopore molecular sieve.It can be seen that its part Cellular structure has been collapsed.
By above content as it can be seen that the synthesis condition of embodiment 1 is optimal.
Embodiment 4
The condition being tentatively carbonized in 1 step 3) of embodiment is changed to 180 DEG C of carbonization 5h.Remaining synthesis condition is constant.
Embodiment 5
The condition calcined in 1 step 5) of embodiment is changed to 600 DEG C of 3 h of calcining.Remaining synthesis condition is constant.
Embodiment 6
The mass fraction of hydrofluoric acid solution in 1 step 6) of embodiment is changed to 25%, soaking time is changed to as 10h.Remaining synthesis item Part is constant.
Embodiment 7
Carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve as active material, with binder Kynoar, conductive agent 80%:10%:5%:5% is mixed and made into electrode pasting by mass percentage for acetylene black and Ketjen black, coated in 1cm × 1cm On carbon cloth collector, electrode to be measured is made in vacuum drying at 75 DEG C, is to electrode with carbon-point, saturated calomel electrode is reference electricity Pole, Mg (NO3)2Aqueous solution is electrolyte, is assembled into traditional three-electrode system, carry out EIS impedance analysis, cyclic voltammetry with And constant current charge-discharge test, corresponding test result are as shown in Figure 5 and Figure 6.It can be seen that its cycle performance is good.
Embodiment 8
Carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve as active material, with binder Kynoar, conductive agent 80%:10%:5%:5% is mixed and made into electrode pasting by mass percentage for acetylene black and Ketjen black, coated in 1cm × 1cm On carbon cloth collector, at 75 DEG C be dried in vacuo be made cathode, with it has been reported that magnesium Mn oxide (Mg-OMS-1/Graphene) Composite material is anode, 0.5 mol dm−3 Mg(NO3)2Aqueous solution is electrolyte, be assembled into the water system magnesium of two electrode systems from Sub- capacitor batteries carry out cyclic voltammetry and constant current charge-discharge test, and test results are shown in figure 7.
Embodiment 9
Carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve as active material, with binder Kynoar, conductive agent 80%:10%:5%:5% is mixed and made into electrode pasting by mass percentage for acetylene black and Ketjen black, coated in 1cm × 1cm On carbon cloth collector, electrode to be measured is made in vacuum drying at 75 DEG C, is to electrode with carbon-point, saturated calomel electrode is reference electricity Pole, NaNO3Aqueous solution is electrolyte, is assembled into traditional three-electrode system；With the Na to have registered0.44MnO2For anode, which is Cathode, 1.0 mol dm−3 NaNO3Water system sodium ion capacitor batteries are assembled into for electrolyte.
Embodiment 10
Carbon prepared by embodiment 1 burns SBA-15 mesopore molecular sieve as active material, with binder Kynoar, conductive agent 80%:10%:5%:5% is mixed and made into electrode pasting by mass percentage for acetylene black and Ketjen black, coated in 1cm × 1cm On carbon cloth collector, electrode to be measured is made in vacuum drying at 75 DEG C, is to electrode with carbon-point, saturated calomel electrode is reference electricity Pole, LiNO3Aqueous solution is electrolyte, is assembled into traditional three-electrode system；With the LiMn to have registered2O4For anode, which is negative Pole, 1.0 mol dm−3 LiNO3Aquo-lithium ion battery is assembled into for electrolyte.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (8)

1. the preparation method that a kind of carbon burns SBA-15 mesopore molecular sieve, it is characterised in that: the following steps are included:
1) concentrated sulfuric acid, sucrose is soluble in water, SBA-15 mesopore molecular sieve is added and is sufficiently mixed, 30min is stirred at room temperature, must mix Liquid；
2) gained mixed liquor is filtered, and is washed with filtrate, filtered 5 ~ 10 times repeatedly, gained filter cake is in 70 DEG C of dry 10h；
3) obtained solid powder after drying is tentatively carbonized, is then ground；
4) with preliminary carbonization and polished black powder alternative steps 1) in SBA-15 mesopore molecular sieve, repeat step 1) ~ 3) it operates 2 times；
5) final gained black powder is calcined under nitrogen protection；
6) calcined black powder is impregnated in hydrofluoric acid solution, to remove template, is washed with water and washs to neutrality to get institute It states carbon and burns SBA-15 mesopore molecular sieve.
2. the preparation method that carbon according to claim 1 burns SBA-15 mesopore molecular sieve, it is characterised in that: step 1) institute In mixed liquor concentrated sulfuric acid content be 0.06 ~ 0.11 g/L, cane sugar content 80g/L, SBA-15 mesopore molecular sieve content is 53 ~ 100 g/L。
3. the preparation method that carbon according to claim 1 burns SBA-15 mesopore molecular sieve, it is characterised in that: described in step 3) The temperature being tentatively carbonized is 150 DEG C ~ 180 DEG C, the time is 5h ~ 8h.
4. the preparation method that carbon according to claim 1 burns SBA-15 mesopore molecular sieve, it is characterised in that: described in step 5) The temperature of calcining is 550 DEG C ~ 750 DEG C, the time is 1h ~ 3h.
5. the preparation method that carbon according to claim 1 burns SBA-15 mesopore molecular sieve, it is characterised in that: used in step 6) The mass fraction of hydrofluoric acid solution is 10% ~ 30%, and soaking time is 10h ~ 30h.
6. carbon made from a kind of method as described in claim 1 burns SBA-15 mesopore molecular sieve.
7. a kind of carbon as claimed in claim 6, which burns SBA-15 mesopore molecular sieve as negative electrode material, is preparing answering in water system battery With.
8. carbon burning SBA-15 mesopore molecular sieve is preparing answering in water system battery as negative electrode material according to claim 7 With, it is characterised in that: its concrete application method are as follows: SBA-15 mesopore molecular sieve is burnt as active material using carbon, Kynoar is Binder, acetylene black and Ketjen black are conductive agent, and by it, 80%:10%:5%:5% forms slurry by mass percentage, by institute It obtains slurry to be coated on carbon cloth collector, is dried in vacuo at 75 DEG C and cathode is made, with LiMn2O4、Na0.44MnO2Or MnO2It is positive Pole, LiNO3、NaNO3Or Mg (NO3)2Aqueous solution is that water system full battery or capacitor batteries are made in electrolyte assembling.
CN201910436494.0A 2019-05-23 2019-05-23 A kind of carbon burns SBA-15 mesopore molecular sieve and preparation method thereof and its application in water system battery Pending CN110155982A (en)

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Publication number Priority date Publication date Assignee Title
CN113845105A (en) * 2021-09-24 2021-12-28 深圳华算科技有限公司 Potassium ion battery negative electrode material, preparation method thereof and potassium ion battery
CN113845105B (en) * 2021-09-24 2023-09-01 深圳华算科技有限公司 Potassium ion battery anode material, preparation method thereof and potassium ion battery

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Application publication date: 20190823