CN107010625B - Waste saccharide liquid prepares the method for porous charcoal ball and prepares electrode slice method with the charcoal ball - Google Patents
Waste saccharide liquid prepares the method for porous charcoal ball and prepares electrode slice method with the charcoal ball Download PDFInfo
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- CN107010625B CN107010625B CN201710377292.4A CN201710377292A CN107010625B CN 107010625 B CN107010625 B CN 107010625B CN 201710377292 A CN201710377292 A CN 201710377292A CN 107010625 B CN107010625 B CN 107010625B
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- charcoal ball
- porous charcoal
- saccharide liquid
- waste saccharide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of methods of waste saccharide liquid preparation porous charcoal ball to be cleaned and dry, four steps of the preparation of porous charcoal ball and the preparation of electrode with the waste saccharide liquid rich in 2-keto-L-gulonic acid generated in vitamin C producing process by hydrothermal carbonization, charcoal ball.The present invention uses waste saccharide liquid for presoma, by hydrothermal carbonization, has synthesized the charcoal ball that surface is rich in oxygen-containing functional group, and activate by KOH, has been prepared for the porous charcoal ball with preferable chemical property.The method realizes the utilization of the high added value to vitamin C waste saccharide liquid produced during the preparation process, and reduces the cost of biopharmaceutical company's processing waste saccharide liquid, also reduces environmental pollution to a certain extent.Also disclosing the charcoal ball prepares electrode slice method simultaneously.
Description
Technical field
The invention belongs to the field of chemical synthesis, and in particular to prepare charcoal ball using a kind of waste saccharide liquid and its by chemical activation
Application in electrochemistry afterwards.
Background technique
Energy shortage is the serious problems that the world today faces, and in order to overcome the problems, such as this, is comprehensively utilized alternative
Lasting renewable resource realize the energy conversion and deposit it is most important.In recent years, fuel cell, battery pack and capacitor etc.
The research of energy reserves technology is concerned.Double layer capacitor is because its energy density is high, have extended cycle life and performance is better than it
Its battery pack, and be widely used in numerous areas.Also, with increasing for production rubbish, waste is handled for convenience, is led
It causes some wastes being recycled by direct emission, has in turn resulted in environmental pollution and the wasting of resources.It is noticeable
It is in ascorbic production process, to produce a large amount of waste saccharide liquid, and contain a large amount of 2-keto-L-gulonic acid, a small amount of
Vitamin C and the alkaline metal ions such as sodium and potassium.Moreover, recycling major embodiment to ascorbic waste liquid at present
Some low value-added products (such as oxalic acid and detergent) are being produced, or recycle 2- ketone group-using more complicated process
L- 2-KLG, prepares vitamin C.
In addition, according to the main composition of waste saccharide liquid it is found that C the and O element of its rich content, is conducive to prepare electrochemistry
It can good active carbon electrode material.In addition to this, some alkaline metal ions in waste saccharide liquid, can play certain activation
Effect.So recycling to waste saccharide liquid, preparing, there is the carbon electrode material of the double layer capacitor of high added value to have
Biggish research significance.
Summary of the invention
The problem to be solved in the present invention is that customer service defect of the existing technology proposes a kind of utilization waste saccharide liquid system
The method of standby porous charcoal ball, while proposing the method for preparing electrode slice with the charcoal ball.It is presoma using waste saccharide liquid, passes through water
Hot carbonization prepares charcoal ball, then carries out pore-creating by chemical activation, and be finally used as the carbon electrode material of double layer capacitor.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
The method that waste saccharide liquid prepares porous charcoal ball, the specific steps of which are as follows:
Step 1, hydrothermal carbonization
Waste saccharide liquid and deionized water are mixed according to the volume ratio of 2:3, to be uniformly mixed them, mixed liquor is carried out
Ultrasonic wave dispersion, ultrasonic dispersing time are the min of 20 min~40,30 min of optimal selection.It is subsequently poured into polytetrafluoroethyl-ne
In the hydrothermal reaction kettle of alkene liner, hydro-thermal process is carried out；Hydrothermal temperature is 140oC~220oC, optimal selection 180oC；Water
The thermal response time is the h of 3 h~15, and the preferably time is 12 h.
After cooled to room temperature, columnar gel Carbon Materials are obtained.
Step 2, the cleaning and drying of charcoal ball
By columnar gel Carbon Materials, ultrasonic wave is first mixed with deionized water and disperses 30 min, then super with ethyl alcohol mixing
30 min of sound, is then filtered, and aforesaid operations are repeated, until filtrate clear, colorless, then by the Carbon Materials after cleaning, it is put in drum
It is dried in wind drying box, obtains charcoal ball, drying condition 80oC、12 h。
Step 3 chemical activation prepares porous charcoal ball
(the mass ratio m after evenly mixing in proportion by charcoal ball and potassium hydroxide (KOH)KOH/mCharcoal ball=0.5~3), in indifferent gas
Atmosphere Ar(argon gas) in activated, activation temperature be 500~750oC, activation time are 1 ~ 3 h.Then, using 2 mol/L's
HCl solution and excessive deionized water are washed and are filtered, until filtrate is in neutrality.Finally, by the charcoal ball after activation cleaning
It places in a vacuum drying oven in 200oC, dry 2 h, obtains porous charcoal ball.
In step 2 and 3, the ethyl alcohol is commercially available analysis straight alcohol, and the hydrochloric acid is the commercially available pure process of analysis
Dilute the dilute hydrochloric acid of 2 mol/L obtained.
The method that a kind of porous charcoal ball by above method preparation proposed by the present invention is used to prepare electrode slice, step
It is:
Step 1, the porous charcoal ball of above method preparation, acetylene black and PTFE are mixed, mass ratio are as follows:
Porous charcoal ball 85%~90%；
Acetylene black 0%~10%；
Polytetrafluoroethylene (PTFE) 0%~5%；
Porous charcoal ball, acetylene black and PTFE optimum quality ratio 87:10:3.
Step 2, said mixture is rolled to thin paper sheet.
Step 3, mixture is depressed into nickel foam, electrode slice is made.
Preferably, it is pressed into the circular electric pole piece that diameter is 13 mm and is impregnated in the KOH solution of 6 mol/L (6 mol/
The KOH solution of L makees electrolyte), it is assembled into double layer capacitor.
Compared with prior art, the present invention has the advantage that
Waste saccharide liquid prepares carbon microspheres by hydrothermal carbonization processing as a kind of novel presoma.Also, waste saccharide liquid is to be in
Liquid does not need to dissolve presoma when carrying out hydro-thermal process.At the same time, it is activated using KOH as activator, it can be with
Increase the specific surface area of carbon microspheres, and generates micropore and mesoporous on charcoal ball.Also, pass through hydrothermal carbonization using waste saccharide liquid,
The charcoal ball surface oxygen-containing functional group rich in of preparation is conducive to the wellability for increasing porous charcoal ball, and counterfeit by increasing
The mode of capacitor increases specific capacitance.
Detailed description of the invention
Fig. 1 be waste saccharide liquid be dried to obtain useless sugar residue, charcoal ball and porous charcoal ball scanning electron microscope (SEM) photograph.A is sweeping for useless sugar residue
Electron microscope is retouched, b, c, d are the scanning electron microscope (SEM) photographs of the charcoal ball under different amplification, and e, f are the porous charcoals under different amplification
The scanning electron microscope (SEM) photograph of ball.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
1 waste saccharide liquid of embodiment prepares porous charcoal ball.
Step 1, waste saccharide liquid is filtered by decompression, removes insoluble impurity, then by the deionized water of 30 mL and 20
After the filtered waste saccharide liquid mixing of mL, carries out ultrasonic wave and disperse 30 min, obtain the mixed solution of 50 mL.
Mixed solution obtained above is poured into the stainless steel hydrothermal reaction kettle of the polytetrafluoroethyllining lining of 100 mL.It will
Hydrothermal reaction kettle is put into air dry oven, 180oAt a temperature of C, after keeping 12 h, cooled to room temperature obtains column
The gel Carbon Materials (dark brown) of shape.
Step 2, by columnar gel Carbon Materials, ultrasonic wave is first mixed with deionized water and disperses 30 min, then and ethyl alcohol
30 min of ultrasound are mixed, are then filtered, aforesaid operations are repeated, up to filtrate clear, colorless, then by the Carbon Materials after cleaning,
It is put in air dry oven and is dried, obtain charcoal ball, drying condition 80oC、12 h。
Step 3, chemical activation prepares porous charcoal ball:
(1) charcoal ball and KOH are mixed in mass ratio: mKOH/mCharcoal ball=1。
(2) it by the mixture of charcoal ball and KOH, is placed in tube furnace, under an ar atmosphere heating (10oC min-1) to setting
Fixed activation temperature 700oC), 2 h are activated.Cooled to room temperature is collected activated material and is sufficiently washed away with 2 mol/L dilute hydrochloric acid
Remaining activator, then be washed with deionized to neutrality, finally 200oDry 2 h, obtain porous charcoal under C vacuum state
Ball.
Step 4, the preparation of electrode slice:
Porous charcoal ball, acetylene black and PTFE prepared by step 3 is mixed according to the mass ratio of 87:10:3, is ground in agate
It is rolled in alms bowl to thin paper sheet, wherein the quality of porous charcoal ball is about 10 mg.Then mixture is depressed into nickel foam, is made
Diameter is the circular electric pole piece of 13 mm.
Finally, the electrode slice made is impregnated in the KOH solution of 6 mol/L, (KOH solution of 6 mol/L is electrolysed
Liquid), and it is assembled into double layer capacitor.
Embodiment 2, it is substantially the same manner as Example 1, except that: ultrasonic dispersing time described in step 1 is 20
min。
Embodiment 3, it is substantially the same manner as Example 1, except that: ultrasonic dispersing time described in step 1 is 40
min。
Embodiment 4, it is substantially the same manner as Example 1, except that: hydrothermal temperature described in step 1 is 140oC。
Embodiment 5, it is substantially the same manner as Example 1, except that: hydrothermal temperature described in step 1 is 160oC。
Embodiment 6, it is substantially the same manner as Example 1, except that: hydrothermal temperature described in step 1 is 200oC。
Embodiment 7, it is substantially the same manner as Example 1, except that: hydrothermal temperature described in step 1 is 220oC。
Embodiment 8, it is substantially the same manner as Example 1, except that: the hydro-thermal reaction time described in step 1 is 3 h.
Embodiment 9, it is substantially the same manner as Example 1, except that: the hydro-thermal reaction time described in step 1 is 6 h.
Embodiment 10, it is substantially the same manner as Example 1, except that: the hydro-thermal reaction time described in step 1 is 9 h.
Embodiment 11, it is substantially the same manner as Example 1, except that: the hydro-thermal reaction time described in step 1 is 15
h。
Embodiment 12, it is substantially the same manner as Example 1, except that: m described in step 3KOH/mCharcoal ball=0.5。
Embodiment 13, it is substantially the same manner as Example 1, except that: m described in step 3KOH/mCharcoal ball=2。
Embodiment 14, it is substantially the same manner as Example 1, except that: m described in step 3KOH/mCharcoal ball=3。
Embodiment 15, it is substantially the same manner as Example 1, except that: activation temperature described in step 3 is 500oC。
Embodiment 16, it is substantially the same manner as Example 1, except that: activation temperature described in step 3 is 600oC。
Embodiment 17, it is substantially the same manner as Example 1, except that: activation temperature described in step 3 is 800oC。
Embodiment 18, it is substantially the same manner as Example 1, except that: activation time described in step 3 is 1 h.
Embodiment 19, it is substantially the same manner as Example 1, except that: activation time described in step 3 is 2.5 h.
Embodiment 21, it is substantially the same manner as Example 1, except that: activation time described in step 3 is 3 h.
The porous charcoal ball of different batches is prepared for the method for the present invention, analysis result is as follows: in mKOH/mCharcoal ball=1, activation temperature
Degree is 700oUnder conditions of C and activation time are 2 h, porous charcoal ball specific surface area with higher (1811 m of preparation2/ g),
Under conditions of current density is 40 mA/g, for specific volume up to 296.11 F/g, energy density is 8.33 Wh/kg.
Claims (6)
1. the method that waste saccharide liquid prepares porous charcoal ball, the specific steps of which are as follows:
Step 1, hydrothermal carbonization
Waste saccharide liquid and deionized water are mixed according to the volume ratio of 2:3, ultrasonic wave dispersion, ultrasonic wave dispersion are carried out to mixed liquor
Time is the min of 20 min~40；It is subsequently poured into hydrothermal reaction kettle, carries out hydro-thermal process, hydrothermal temperature is 140 DEG C~220
DEG C, the hydro-thermal reaction time is the h of 3 h~15；After cooled to room temperature, columnar gel Carbon Materials are obtained；
The waste saccharide liquid is the waste saccharide liquid generated in vitamin C producing process, and containing 2-keto-L-gulonic acid, vitamin C with
And sodium and potassium alkaline metal ions；
Step 2, the cleaning and drying of charcoal ball
By columnar gel Carbon Materials, ultrasonic wave is first mixed with deionized water and disperses 30 min, then mix ultrasound 30 with ethyl alcohol
Then min is filtered, aforesaid operations are repeated, until filtrate clear, colorless, then by the Carbon Materials after cleaning, it is dry to be put in air blast
It is dried in dry case, obtains charcoal ball；
Step 3 chemical activation prepares porous charcoal ball
By charcoal ball and potassium hydroxide 1:1 in mass ratio mix, in inert atmosphere Ar(argon gas) in activated, activation temperature is
700~750 DEG C, activation time is 2~3 h；Then, it is washed using the HCl solution of 2 mol/L and excessive deionized water
It washs and filters, until filtrate is in neutrality；Finally, the charcoal ball after activation cleaning is dry, obtain porous charcoal ball.
2. the method for waste saccharide liquid preparation porous charcoal ball according to claim 1, it is characterized in that: ultrasound wavelength-division described in step 1
Dissipating the time is 30 min, and hydrothermal temperature is 180 DEG C, and the hydro-thermal reaction time is 12 h.
3. the method for waste saccharide liquid preparation porous charcoal ball according to claim 1, it is characterized in that: activation temperature described in step 3
It is 700 DEG C, activation time 2h.
4. the method for waste saccharide liquid preparation porous charcoal ball according to claim 1, it is characterized in that: the ethyl alcohol is to analyze pure second
Alcohol, the hydrochloric acid are 2 mol/L dilute hydrochloric acid.
5. a kind of method that the porous charcoal ball prepared with one of claim 1-4 the method prepares electrode slice, the steps include:
Step 1, the porous charcoal ball of above method preparation, acetylene black and PTFE are mixed, mass ratio are as follows:
Porous charcoal ball 85%~90%；
Acetylene black 0%~10%；
Polytetrafluoroethylene (PTFE) 0%~5%；
Step 2, said mixture is rolled to thin paper sheet；
Step 3, mixture is depressed into nickel foam, electrode slice is made.
6. the porous charcoal ball according to claim 5 prepared with one of claim 1-4 the method prepares electrode slice
Method, it is characterized in that: the porous charcoal ball, acetylene black and PTFE mass ratio are 87:10:3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109095451A (en) * | 2018-07-23 | 2018-12-28 | 昆明理工大学 | A kind of expired useless medicine vitamin B1The recoverying and utilizing method of injection |
| CN109052395A (en) * | 2018-09-13 | 2018-12-21 | 中国矿业大学 | Waste saccharide liquid prepares the method for tremelliform porous charcoal and is used to prepare electrode slice |
| CN110357061B (en) * | 2018-09-25 | 2022-12-23 | 昆明理工大学 | Recovery method of overdue waste drug acute bronchitis particles |
| CN110911741B (en) * | 2019-12-10 | 2021-05-25 | 中国石油大学(北京) | Carbon oxide sphere doped solid polymer electrolyte membrane and preparation method and application thereof |
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| CN101538034A (en) * | 2009-04-24 | 2009-09-23 | 江苏大学 | Preparation method of one-step synthesis carbon ball |
| CN103785371A (en) * | 2014-03-04 | 2014-05-14 | 湘潭大学 | Porous carbon microsphere @TiO2 composite material and preparation method and application thereof |
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| CN101538034A (en) * | 2009-04-24 | 2009-09-23 | 江苏大学 | Preparation method of one-step synthesis carbon ball |
| CN103785371A (en) * | 2014-03-04 | 2014-05-14 | 湘潭大学 | Porous carbon microsphere @TiO2 composite material and preparation method and application thereof |
| CN106276843A (en) * | 2015-05-12 | 2017-01-04 | 北京化工大学 | A kind of method preparing monodisperse hollow carbon microspheres |
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