CN106953112B - A kind of three-diemsnional electrode material preparation method and application - Google Patents
A kind of three-diemsnional electrode material preparation method and application Download PDFInfo
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- CN106953112B CN106953112B CN201710321192.XA CN201710321192A CN106953112B CN 106953112 B CN106953112 B CN 106953112B CN 201710321192 A CN201710321192 A CN 201710321192A CN 106953112 B CN106953112 B CN 106953112B
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- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
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Abstract
The present invention provides a kind of preparation method of three-diemsnional electrode material, comprising the following steps: impregnates luffa in prepared Chinese ink, then takes out and be dried, repeat to impregnate and dry step 2~4 time, obtains three-diemsnional electrode material.The present invention is based on the excellent electric conductivity of prepared Chinese ink and good adhesion strengths, and luffa fibre structure abundant and bigger serface are easy to the advantages that microorganism attachment, prepared Chinese ink is coated on luffa and prepares a kind of three-diemsnional electrode material based on ink conductive layer, and microorganism electrochemical electricity production system biological anode material can be applied to.The process facilitate it is simple and direct, without expensive equipment, it is a kind of electrode preparation method efficiently, cheap, environmentally friendly, it is also a kind of paint-on technique of novelty, provides new approaches for efficient utilize of conventional substances, while also providing a kind of new method for the preparation of three-diemsnional electrode material.The present invention also provides a kind of application of three-diemsnional electrode material and above-mentioned three-diemsnional electrode material in microorganism electrochemical system.
Description
Technical field
The invention belongs to battery technology and environment protection field more particularly to a kind of three-diemsnional electrode material preparation method and applications.
Background technique
Microorganism electrochemical system (Microbial bioelectrochemical system abbreviation BES) technology is close
A kind of new technology for having merged sewage treatment and biology electricity production developed rapidly in year, it can be received while handling sewage
Electric energy is obtained, therefore is widely paid close attention to, microorganism electrochemical system is using the bacterium on anode as anode catalyst, bacterium drop
Electron-transport caused by organic matter is solved to anode, then is loaded by external circuit and reaches cathode, thus generates extrinsic current, bacterium drop
It solves proton caused by organic matter and reaches cathode from anode chamber's reduction of fractions to a common denominator barrier material, reacted on cathode with electronics, oxygen and generate water,
To complete the transmitting of charge in battery.Currently, the electricity generation ability of microorganism electrochemical system is also very low, still have from practical application
Biggish distance, therefore, how to improve the anode electricity generation performance of microorganism electrochemical system is the research hotspot in the field.
From the point of view of the composition of BES, anode bears the effect that microorganism adheres to and transmits electronics, is to determine BES electricity production energy
The important auxiliary tool of an important factor for power and microorganisms electricity production mechanism and electron mechanism, therefore, to BES sun
The research of pole has a very important significance.
Currently, the anode of microorganism electrochemical system is mainly using carbon as made of substrate, including carbon paper, carbon cloth, graphite
Piece (stick) and carbon felt etc..But the electricity generation performance of these materials all need to be improved.
Summary of the invention
A kind of three-dimensional the purpose of the present invention is to provide three-diemsnional electrode material, preparation method and application, in the present invention
Electrode material cost is cheap, and electricity generation performance with higher.
The present invention provides a kind of preparation method of three-diemsnional electrode material, comprising the following steps:
Luffa is impregnated in prepared Chinese ink, then takes out and is dried, repeats to impregnate and dry step 2~4 time, is obtained
Three-diemsnional electrode material.
Preferably, the water content of the luffa is 3~8%.
Preferably, the time of the immersion is 30~40min.
Preferably, it after the luffa after taking out the immersion, is first hung, is then dried again.
Preferably, the time of the suspension is 3~5min.
Preferably, the temperature of the drying is 60~80 DEG C;
The time of the drying is 1~3 hour.
Preferably, the luffa first follows the steps below pretreatment before immersion:
The luffa is impregnated 1~2 hour in water, then successively carries out ultrasonic cleaning 2~3 times with water and ethyl alcohol, most
After dried, obtain pretreated luffa.
Preferably, the temperature of the drying is 60~80 DEG C.
The present invention provides a kind of three-diemsnional electrode material, is made according to the preparation method in claim 1~8.
The present invention also provides application of the above-mentioned three-diemsnional electrode material in microorganism electrochemical system.
The present invention provides a kind of preparation method of three-diemsnional electrode material, comprising the following steps: soaks luffa in prepared Chinese ink
It steeps, then take out and be dried, repeat to impregnate and dry step 2~4 time, obtain three-diemsnional electrode material.The present invention is based on ink
It is attached that the excellent electric conductivity of juice and good adhesion strength and luffa fibre structure abundant and bigger serface are easy to microorganism
The advantages that, prepared Chinese ink is coated on luffa and prepares a kind of three-diemsnional electrode material based on ink conductive layer, and can be applied
In microorganism electrochemical system biological anode material.The process facilitate it is simple and direct, without expensive equipment, be it is a kind of efficiently, cheap, ring
The electrode preparation method of guarantor and a kind of paint-on technique of novelty provide new approaches for efficient utilize of conventional substances, simultaneously
Also the preparation for three-diemsnional electrode material provides a kind of new method.Three-diemsnional electrode material in the present invention can be applied to microorganism electricity
Chemical system is as anode material, and current time response curve has high current under three-electrode system, and electricity generation performance is better than
Carbon felt electrode.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the photo of coating 5 times three-diemsnional electrode materials in the embodiment of the present invention 1;
Fig. 2 is the impedance curve of the three-diemsnional electrode material of different coating numbers in the embodiment of the present invention 1;
Fig. 3 is the impedance curve of the three-diemsnional electrode material in the embodiment of the present invention 1~3;
Fig. 4 is the current time response curve of microorganism electrochemical system and carbon felt electrode in the embodiment of the present invention 4.
Specific embodiment
The present invention provides a kind of preparation methods of three-diemsnional electrode material, comprising the following steps:
Luffa is impregnated in prepared Chinese ink, then takes out and is dried, repeats to impregnate and dry step 2~4 time, is obtained
Three-diemsnional electrode material.
Three-diemsnional electrode material in the present invention is a kind of porous three-dimensional using ink as conductive layer, natural loofah for substrate
Electrode material, can be applied to microorganism electrochemical system is anode material, and current time response curve has under three-electrode system
There is high current, is a kind of good anode material.
The present invention preferably pre-processes luffa, and then pretreated luffa is carried out again to subsequent immersion, done
The processing steps such as dry.Pretreatment in the present invention is preferably cleaned, and the present invention preferably impregnates luffa 1~2 hour in water,
Luffa surface impurity is removed, then successively spends water and ethyl alcohol carries out ultrasonic cleaning 2~3 times, removal luffa is intrapore stupid
Gu impurity is finally dried, pretreated luffa is obtained.
Present invention preferably employs thick matter luffa, the water content of the luffa is preferably 3~8%, more preferably 4~
7%, most preferably 5~6%.The present invention does not have special limitation to the source of the luffa.The present invention is preferably by the silk
Melon network is trimmed to the three-dimensional bulk of 1cm × 1cm × 0.5cm shape, is then fixed in titanium silk one end as three-diemsnional electrode.
In the present invention, the water of the immersion is preferably deionized water, and water used in the ultrasonic cleaning is preferably gone
Ionized water, being cleaned by ultrasonic ethyl alcohol used is preferably dehydrated alcohol, and the time of the ultrasonic cleaning is preferably 20~30min, institute
The temperature for stating drying is preferably 60~80 DEG C, more preferably 65~75 DEG C, most preferably 70 DEG C;The time of the drying is preferably
1~3 hour, more preferably 2 hours.
After the pretreatment for completing luffa, the present invention preferably impregnates pretreated luffa in prepared Chinese ink, then takes out
It is dried, repeats immersion and dry step 2~4 time, obtain three-diemsnional electrode material.The present invention is preferably by pretreated sponge gourd
Network impregnates in prepared Chinese ink, then takes out suspension, and the prepared Chinese ink drip for absorbing luffa is to the greatest extent and unlikely luffa gap blocks, most laggard
Row drying makes prepared Chinese ink be fixed on luffa surface, and repeating this process of immersion-suspension-drying 2~4 times, (i.e. immersion-suspension-is dry
This dry process is implemented 3~5 times altogether), obtain three-diemsnional electrode material.
In the present invention, the prepared Chinese ink preferably uses Guangzhou Zhujiang board prepared Chinese ink, the red apple of Hunan Hunan word board prepared Chinese ink and Shandong
One or more of fruit board prepared Chinese ink, the present invention does not have special limitation to the dosage of the prepared Chinese ink, can be by the luffa
It is totally submerged.In an embodiment of the present invention, the prepared Chinese ink of 100~200mL can be used.The time of the immersion is preferably 30
~40min;The present invention preferably shakes luffa 3~5 times back and forth in prepared Chinese ink, is substantially adhered to prepared Chinese ink on luffa;Institute
The time for stating suspension is preferably 3~5min;The present invention is drained extra prepared Chinese ink by hanging, and luffa is made to be coated with prepared Chinese ink
While be also able to maintain three-dimensional porous structure, so as to the attachment of subsequent microorganism.The temperature of the drying is preferably 60~80
DEG C, more preferably 65~75 DEG C, most preferably 70 DEG C;The time of the drying is preferably 1~3 hour, and more preferably 2 hours.
The present invention preferably by immersion-suspension-drying, implemented 3 times, 4 times or 5 times altogether by this process, to obtain more preferable electric conductivity
The three-diemsnional electrode material of energy.
The present invention provides a kind of three-diemsnional electrode materials, and preparation method as described above is made.
The present invention also provides a kind of application of three-diemsnional electrode material as described above in microorganism electrochemical system.
Three-diemsnional electrode material in the present invention is applied in microorganism electrochemical system as anode material, specifically, can
It applies in microbiological fuel cell.It in an embodiment of the present invention, can be using the three-diemsnional electrode material in the present invention as work
Electrode, titanium silk volume are auxiliary electrode, and saturated calomel electrode is public reference electrode, construct three-electrode system microorganism electrochemical system
System.In the three electrodes microorganism electrochemical system, it is preferred to use anaerobism mixed bacteria liquid and sodium acetate substrate solution are placed in
It is cultivated in 30 ± 1 DEG C of environment, the sodium acetate substrate solution is at being grouped as are as follows: NaH2PO4·2H2O(2.77g·L-1)、
Na2HPO4·12H2O(11.40g·L-1)、NH4Cl(0.31g·L-1)、KCl(0.13g·L-1), vitamin solution (10mLL-1) and mineral solution (10mLL-1)。
The present invention provides a kind of preparation method of three-diemsnional electrode material, comprising the following steps: soaks luffa in prepared Chinese ink
It steeps, then take out and be dried, repeat to impregnate and dry step 3~5 time, obtain three-diemsnional electrode material.The present invention is based on ink
It is attached that the excellent electric conductivity of juice and good adhesion strength and luffa fibre structure abundant and bigger serface are easy to microorganism
The advantages that, prepared Chinese ink is coated on luffa and prepares a kind of three-diemsnional electrode material based on ink conductive layer, and can be applied
In microorganism electrochemical system biological anode material.The process facilitate it is simple and direct, without expensive equipment, be it is a kind of efficiently, cheap, ring
The electrode preparation method of guarantor and a kind of paint-on technique of novelty provide new approaches for efficient utilize of conventional substances, simultaneously
Also the preparation for three-diemsnional electrode material provides a kind of new method.Three-diemsnional electrode material in the present invention can be applied to microorganism electricity
Chemical system is as anode material, and current time response curve has high current under three-electrode system, and electricity generation performance is better than
Carbon felt electrode.
In order to further illustrate the present invention, with reference to embodiments to a kind of three-diemsnional electrode material provided by the invention, its
Preparation method and application is described in detail, but cannot be understood as limiting the scope of the present invention.
Embodiment 1
1) three-dimensional for luffa being trimmed to 1 × 1 × 0.5cm (length × width x thickness) size is blocky, and is securely fixed
A three-diemsnional electrode is made as in one end of titanium silk;
2) 100mL Guangzhou Zhujiang board calligraphy prepared Chinese ink is taken, above-mentioned electrode is all immersed in prepared Chinese ink and is shaken 5 times back and forth,
Standing 30min afterwards fully absorbs it.It is then taken out suspension 3min, drains 60 DEG C of dry 2h after prepared Chinese ink.
3) step 2) is repeated twice respectively, 3 times and 4 times, three based on ink conductive layer of different coating numbers is made
Tie up electrode material.
Three-diemsnional electrode material high definition photo such as Fig. 1 manufactured in the present embodiment based on ink conductive layer shows that Fig. 1 is the present invention
The photo of coating 5 times three-diemsnional electrode materials in embodiment 1.In Fig. 1, left figure is the luffa of uncoated ink layer, right figure
For the luffa for being coated with 5 ink layers.
3 times, 4 times and 5 times three-diemsnional electrode materials will be coated with altogether in the present embodiment in neutral phosphate buffer solution
Its impedance curve is tested, as a result as shown in Fig. 2, Fig. 2 is the three-diemsnional electrode material of different coating numbers in the embodiment of the present invention 1
Impedance curve, impedance include that the resistance of material and induction reactance two parts parameter, impedance curve can be shown that the size of material resistance characteristic.
Wherein half-round curve is smaller, then shows that electrode charge transfger impedance is lower, electrodes conduct performance is better.As seen from Figure 2, it applies
The electric conductivity for covering 5 three-diemsnional electrode materials is best.
Embodiment 2
1) three-dimensional for luffa being trimmed to 1 × 1 × 0.5cm (length × width x thickness) size is blocky, and is securely fixed
A three-diemsnional electrode is made as in one end of titanium silk;
2) Hunan 100mL Hunan word board calligraphy prepared Chinese ink is taken, above-mentioned electrode is all immersed in prepared Chinese ink and is shaken 5 times back and forth,
Standing 30min afterwards fully absorbs it.It is then taken out suspension 5min, drains 80 DEG C of dry 2h after prepared Chinese ink.
3) step 2) is repeated 4 times, obtains the three-diemsnional electrode material based on ink conductive layer.
Embodiment 3
1) three-dimensional for luffa being trimmed to 1 × 1 × 0.5cm (length × width x thickness) size is blocky, and is securely fixed
A three-diemsnional electrode is made as in one end of titanium silk;
2) Shandong 100mL red apple board calligraphy prepared Chinese ink is taken, above-mentioned electrode is all immersed in prepared Chinese ink and shakes 5 back and forth
Secondary, the rear 30min that stands fully absorbs it.It is then taken out suspension 5min, drains 80 DEG C of dry 2h after prepared Chinese ink.
3) step 2) is repeated 4 times, obtains the three-diemsnional electrode material based on ink conductive layer.
The present invention will coat 5 three-diemsnional electrode materials, the three-diemsnional electrode material in embodiment 2~3 in embodiment 1
Its impedance curve is tested in acid phosphate buffer solution, as a result as shown in figure 3, Fig. 3 is the three-dimensional in the embodiment of the present invention 1~3
The impedance curve of electrode material.As seen from Figure 3, the three-dimensional electricity of Zhujiang River board calligraphy prepared Chinese ink has been used in EXAMPLE Example 1
Pole materials conductive performance is best.
Embodiment 4
The building of three-electrode system microorganism electrochemical system
By conventional titanium silk one end around the web-like for diameter 1cm, long 3cm, 3 auxiliary electrodes are made;
Using 500mL transparent plastic sealing vessel as battery case, 5 luffa electrodes are coated in embodiment 1 respectively
With what gloomy carbon felt electrode of the Shanghai of purchase be working electrode, titanium silk volume is auxiliary electrode, saturated calomel electrode is public reference electricity
Pole constructs 2 three-electrode system microorganism electrochemical systems.
For the microorganism electrochemical system of building in addition to anode material is different from the routine BES of three-electrode system, other are homogeneous
Together.
The operation of microorganism electrochemical system
250ml anaerobism mixed bacteria liquid and 250ml sodium acetate (1000mg are inoculated with into the above-mentioned BES system being equipped with
L-1) substrate solution is placed in 30 ± 1 DEG C of environment and cultivates, and each electrode is serially connected to electrochemical workstation (Shanghai occasion
China, CHI1040C) to detect current time response curve.Sodium acetate substrate solution is at being grouped as are as follows: NaH2PO4·2H2O
(2.77g·L-1)、Na2HPO4·12H2O(11.40g·L-1)、NH4Cl(0.31g·L-1)、KCl(0.13g·L-1), vitamin
Solution (10mLL-1) and mineral solution (10mLL-1)。
The current time response curve of microorganism electrochemical system is as shown in figure 4, Fig. 4 is that the present invention is implemented in the present embodiment
The current time response curve of microorganism electrochemical system and carbon felt electrode in example 4, current time response curve are to record micro- life
Object generates electric current versus time curve on the electrode, and electrode performance height can be directly judged according to size of current.Current value
Bigger, then electrode performance is better.As shown in Figure 4, when the three-diemsnional electrode material in embodiment 1 is applied to microorganism electrochemical system
Current value be much larger than common carbon felt electrode, have better electrode performance.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of three-diemsnional electrode material, comprises the steps of:
Luffa is impregnated 1~2 hour in water, then successively carried out ultrasonic cleaning 2~3 times with water and ethyl alcohol, is finally dried
It is dry, obtain pretreated luffa;The temperature of the drying is 60~80 DEG C;
Luffa is impregnated in prepared Chinese ink, is first hung, is then dried, repetition immersion, suspension and dry step 2~
4 times, obtain three-diemsnional electrode material;
The temperature of the drying is 60~80 DEG C;The time of the drying is 1~3 hour.
2. preparation method according to claim 1, which is characterized in that the water content of the luffa is 3~8%.
3. preparation method according to claim 1, which is characterized in that the time of the immersion is 30~40min.
4. preparation method according to claim 1, which is characterized in that the time of the suspension is 3~5min.
5. a kind of three-diemsnional electrode material is made according to the preparation method in Claims 1 to 4.
6. application of the three-diemsnional electrode material in microorganism electrochemical system described in claim 5.
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CN108252081B (en) * | 2018-01-03 | 2020-06-16 | 江苏理工学院 | Preparation method and application of loofah sponge/carbon-based nanoparticle synergistically modified polymer conductive composite material |
CN110350210A (en) * | 2019-07-26 | 2019-10-18 | 哈尔滨工业大学 | A kind of preparation method for the anode of microbial fuel cell loading MXene on carbonization luffa |
CN112903438A (en) * | 2021-01-21 | 2021-06-04 | 常州工学院 | Loofah sponge/liquid metal-based sensor and preparation method thereof |
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