CN107591540A - A kind of preparation method of biological fuel cell anode material - Google Patents
A kind of preparation method of biological fuel cell anode material Download PDFInfo
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- CN107591540A CN107591540A CN201710746438.8A CN201710746438A CN107591540A CN 107591540 A CN107591540 A CN 107591540A CN 201710746438 A CN201710746438 A CN 201710746438A CN 107591540 A CN107591540 A CN 107591540A
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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
Abstract
The present invention discloses a kind of preparation method of biological fuel cell anode material, with graphene and polyaniline-modified traditional anode material carbon cloth, single-layer graphene oxide is first modified with styrene sulfonic acid, then hydrophilic graphene is obtained with hydrazine hydrate reduction single-layer graphene oxide again, by hydrophilic graphene add containing aniline monomer, initiator, pore-foaming agent composite solution in, again by composite solution coated on the carbon cloth through hydrophilic pretreatment, composite solution reacts on carbon cloth, is then dried to obtain anode material.The biological fuel cell anode material that the present invention prepares has the advantages of biological attachment area is big, hydrophilicity is good, electric conductivity is strong, electricity generation performance is good.
Description
Technical field
The invention belongs to biological fuel cell field, and in particular to a kind of preparation side of biological fuel cell anode material
Method.
Background technology
Biological fuel cell is a kind of device that chemical energy is converted into electric energy using biocatalyst, utilizes micro- life
Thing metabolic process carries with the research and development for the biological fuel cell that electrode reaction is combined for production of renewable energy resources and offal treatment
A new way is supplied.Biological fuel cell is by the use of microorganism as reactive agent, by the chemical energy of fuel (organic substance)
Be converted into electric energy, it be it is a kind of using it is various biology be used as catalyst devices, conventional biocatalyst have microorganism, carefully
Born of the same parents' device (such as mitochondria) and enzyme, its type are determined by the species of biocatalyst.
Carrier of the anode of biological fuel cell as electricity production biological attachment, the adhesion amount of electricity production biology is not only influenceed, together
When have an effect on transmission of the electronics from microorganism to anode, on improve battery electricity generation performance have vital influence.It is high performance
Biological fuel cell anode requirement is easy to electricity-producing microorganism apposition growth, is easy to electron transmission, while require anode interior resistance
It is small, electric conductivity is strong, anode potential is stable.The electricity generation performances such as current traditional carbon paper, carbon cloth, graphite cake, soft graphite are general, work(
Rate problem becomes the bottleneck for influenceing biological fuel cell development.
The content of the invention
The present invention provides a kind of preparation method of biological fuel cell anode material, by changing to traditional carbon cloth anode
Property, prepare the anode material that biological attachment area is big, hydrophilicity is good, electric conductivity is strong, electricity generation performance is good.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of preparation method of biological fuel cell anode material, comprises the following steps：
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 5~8 parts of styrene sulfonic acids and 100 parts of deionized waters are mixed
Close, 24h is stirred at room temperature, then add 5~7 parts of hydrazine hydrates, flow back 8~12h at 90~95 DEG C, then filtration washing,
Solid product is dried in vacuo, obtains hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.3~0.9 part of hydrophilic graphene, 1~5 part of acrylic acid
Monomer, 30~40 parts of aniline monomers are added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1~1.5, use ice-water bath
It is 0~5 DEG C to control temperature of reactor, with 400~500r/min rotating speed mechanical agitation, then adds 0.25~0.3 part of initiation
Agent, 1~3 part of pore-foaming agent, obtains composite solution；
S3. composite solution is uniformly coated on carbon cloth surfaces, 1~2h is reacted at room temperature, then at 55~60 DEG C
Drying, then alternately rinsed with deionization and acetone, finally obtain anode material.
Further, the carbon cloth is by pretreatment, preprocess method：Carbon cloth is immersed in ethanol or acetone soln
In, then 0.5~1h of ultrasonic vibration, then takes out and dries, be then placed in concentration be 20~30% hydrogen peroxide in immersion 6~
8h, rinsed and then dried standby with water.
Further, the composite solution is coated in carbon cloth surfaces in 15min.
Further, the pore-foaming agent is the quality of the mixture of sodium carbonate and sodium acid carbonate, sodium carbonate and sodium acid carbonate
Than for 1:0.5~1.3.
Further, the initiator is any one in ammonium persulfate, potassium peroxydisulfate, ammonium persulfate/sodium sulfite,
The molal weight of ammonium persulfate and sodium sulfite ratio is 1 in ammonium persulfate/sodium sulfite:0.1~0.3.
Beneficial effects of the present invention：
(1) present invention carrys out modification carbon cloth with hydrophilic graphene and polyaniline, and graphene has more compared with carbon cloth
Good biocompatibility and electric conductivity, and the specific surface area of graphene is bigger than carbon cloth, is more beneficial for the attachment surface of increase biology
Product, the present invention carry out hydrophilic treated to graphene so that graphene is evenly distributed in the solution, and aniline monomer of the present invention is in sulfonic acid
Lower polymerization, obtains partly sulfonated polyaniline, so as to increase the hydrophilic radical on polyaniline surface, strengthens the hydrophily of polyaniline, this
The carbon cloth of invention passes through hydrophilic pretreatment, improves the hydrophilicity of carbon cloth, therefore anode material hydrophilicity prepared by the present invention
It is good, be advantageous to the attachment and growth of biology.
(2) present invention adds pore-foaming agent in composite solution, and pore-foaming agent can produce gas during monomer polymerize
Body so that duct is formed in polymer, duct can increase the surface area of polymer, while can also increase the energy of adsorption of polymer
Power so that anode material can adhere to more biologies, while also improve fixed effect of the biology on anode material.
(3) contain acrylic acid in composite solution of the invention, be on the one hand used for the hydrophilicity for improving polymer, the opposing party
Face is advantageous to increase the viscosity and plasticity of composite solution so that combines more firmly between composite solution and carbon cloth, while also has
Beneficial to thickness of the control composite solution after carbon cloth surfaces shaping.
(4) carbon cloth of the invention, which applies, is covered with composite solution and reacts 1~2h at room temperature so that monomer polymerize, then 55
Drying is on the one hand to moisture removal at~60 DEG C, is on the other hand to decompose remnants sodium acid carbonate, reduces anode material
Impurity in material.
(5) the uncoated preceding temperature of composite solution of the present invention is 0~5 DEG C, and polymerization rate is slow, is coated in composite solution
The process of carbon cloth surfaces reserves time enough, and composite solution is coated in carbon cloth surfaces in 15min, avoids composite solution not
With regard to overreaction before coating, it is unfavorable for subsequent coated process, the sulfonic acid acidifying carbon cloth in composite solution is advantageous to further improve
The hydrophily of carbon cloth.
(6) the practical pore-foaming agent of the present invention is sodium carbonate and the mixture of sodium acid carbonate, can by both ratios come
Adjust speed caused by gas so that the hole of sufficient amount is formed when polyaniline is molded, gas generation is too fast easily to cause gas
Runaway, the duct of formation is excessive, forms excessive velocities easily causes duct to cave in, and gas produced then to be not easy to form hole slowly.
(7) when the present invention using ammonium persulfate/sodium sulfite is initiator, the amount of sodium sulfite can influence the speed reacted
Degree, sodium sulfite can excessively cause polymerisation too fast, be unfavorable for the coating of composite solution.
Embodiment
For ease of more fully understanding the present invention, it is illustrated by following instance, these examples belong to the protection of the present invention
Scope, but do not limit the scope of the invention.
Embodiment 1
A kind of preparation method of biological fuel cell anode material, comprises the following steps：
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 5 parts of styrene sulfonic acids and 100 parts of deionized waters mixed,
24h is stirred at room temperature, then adds 5 parts of hydrazine hydrates, flow back 10h at 95 DEG C, then filtration washing, by solid product vacuum
Dry, obtain hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.6 part of hydrophilic graphene, 3 parts of acrylic monomers, 30
Part aniline monomer is added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1, controls the temperature of reactor to be with ice-water bath
2 DEG C, with 430r/min rotating speed mechanical agitation, 0.25 part of initiator is then added, 3 parts of pore-foaming agents, obtains composite solution；
S3. carbon cloth is immersed in ethanol or acetone soln, then ultrasonic vibration 1h, then takes out and dry, be then placed in
Concentration is to soak 7h in 25% hydrogen peroxide, is rinsed with water and then dries to obtain pretreatment carbon cloth.
S4., composite solution is uniformly coated on to pretreatment carbon cloth surfaces in 15min, reacts 1.5h at room temperature, so
Dry at 55 DEG C, then alternately rinsed with deionization and acetone afterwards, finally obtain anode material.
The pore-foaming agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:1.3.
The initiator is ammonium persulfate/sodium sulfite, ammonium persulfate and sodium sulfite in ammonium persulfate/sodium sulfite
Molal weight ratio is 1:0.1.
Embodiment 2
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 8 parts of styrene sulfonic acids and 100 parts of deionized waters mixed,
24h is stirred at room temperature, then adds 7 parts of hydrazine hydrates, flow back 12h at 92 DEG C, then filtration washing, by solid product vacuum
Dry, obtain hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.3 part of hydrophilic graphene, 5 parts of acrylic monomers, 35
Part aniline monomer is added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1.5, and temperature of reactor is controlled with ice-water bath
For 5 DEG C, with 400r/min rotating speed mechanical agitation, 0.3 part of initiator is then added, 1 part of pore-foaming agent, obtains composite solution；
S3. carbon cloth is immersed in ethanol or acetone soln, then ultrasonic vibration 0.5h, then takes out and dry, Ran Houfang
Enter in the hydrogen peroxide that concentration is 30% and soak 6h, rinsed with water and then dry to obtain pretreatment carbon cloth.
S4., composite solution is uniformly coated on to pretreatment carbon cloth surfaces in 15min, reacts 1h at room temperature, then
Dry at 60 DEG C, then alternately rinsed with deionization and acetone, finally obtain anode material.
The pore-foaming agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:0.5.
The initiator is ammonium persulfate/sodium sulfite, ammonium persulfate and sodium sulfite in ammonium persulfate/sodium sulfite
Molal weight ratio is 1:0.3.
Embodiment 3
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 6 parts of styrene sulfonic acids and 100 parts of deionized waters mixed,
24h is stirred at room temperature, then adds 6.5 parts of hydrazine hydrates, flow back 8h at 90 DEG C, and then filtration washing, true by solid product
Sky is dried, and obtains hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.9 part of hydrophilic graphene, 1 part of acrylic monomers, 40
Part aniline monomer is added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1.2, and temperature of reactor is controlled with ice-water bath
For 0 DEG C, with 500r/min rotating speed mechanical agitation, 0.28 part of initiator is then added, 2 parts of pore-foaming agents, obtains composite solution；
S3. carbon cloth is immersed in ethanol or acetone soln, then ultrasonic vibration 0.8h, then takes out and dry, Ran Houfang
Enter in the hydrogen peroxide that concentration is 20% and soak 8h, rinsed with water and then dry to obtain pretreatment carbon cloth.
S4., composite solution is uniformly coated on to pretreatment carbon cloth surfaces in 15min, reacts 2h at room temperature, then
Dry at 58 DEG C, then alternately rinsed with deionization and acetone, finally obtain anode material.
The pore-foaming agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:0.9.
The initiator is ammonium persulfate/sodium sulfite, ammonium persulfate and sodium sulfite in ammonium persulfate/sodium sulfite
Molal weight ratio is 1:0.2.
Embodiment 4
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 5 parts of styrene sulfonic acids and 100 parts of deionized waters mixed,
24h is stirred at room temperature, then adds 6.8 parts of hydrazine hydrates, flow back 12h at 93 DEG C, and then filtration washing, true by solid product
Sky is dried, and obtains hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.9 part of hydrophilic graphene, 1 part of acrylic monomers, 36
Part aniline monomer is added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1, controls the temperature of reactor to be with ice-water bath
1 DEG C, with 500r/min rotating speed mechanical agitation, 0.27 part of initiator is then added, 2 parts of pore-foaming agents, obtains composite solution；
S3. carbon cloth is immersed in ethanol or acetone soln, then ultrasonic vibration 1h, then takes out and dry, be then placed in
Concentration is to soak 8h in 30% hydrogen peroxide, is rinsed with water and then dries to obtain pretreatment carbon cloth.
S4., composite solution is uniformly coated on to pretreatment carbon cloth surfaces in 15min, reacts 2h at room temperature, then
Dry at 59 DEG C, then alternately rinsed with deionization and acetone, finally obtain anode material.
The pore-foaming agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:0.4.
The initiator is ammonium persulfate.
Embodiment 5
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 8 parts of styrene sulfonic acids and 100 parts of deionized waters mixed,
24h is stirred at room temperature, then adds 6.5 parts of hydrazine hydrates, flow back 11h at 95 DEG C, and then filtration washing, true by solid product
Sky is dried, and obtains hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.8 part of hydrophilic graphene, 4 parts of acrylic monomers, 38
Part aniline monomer is added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1, controls the temperature of reactor to be with ice-water bath
2 DEG C, with 400r/min rotating speed mechanical agitation, 0.28 part of initiator is then added, 3 parts of pore-foaming agents, obtains composite solution；
S3. carbon cloth is immersed in ethanol or acetone soln, then ultrasonic vibration 0.8h, then takes out and dry, Ran Houfang
Enter in the hydrogen peroxide that concentration is 30% and soak 8h, rinsed with water and then dry to obtain pretreatment carbon cloth.
S4., composite solution is uniformly coated on to pretreatment carbon cloth surfaces in 15min, reacts 2h at room temperature, then
Dry at 60 DEG C, then alternately rinsed with deionization and acetone, finally obtain anode material.
The pore-foaming agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:0.5.
The initiator is potassium peroxydisulfate.
Comparative example 1
S1. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.3 part of graphene, 5 parts of acrylic monomers, 35 parts of aniline
Monomer is added in reactor of the dress by the hydrochloric acid solution that 300 parts of pH value are 1.5, and it is 5 DEG C to control temperature of reactor with ice-water bath,
With 400r/min rotating speed mechanical agitation, 0.3 part of initiator is then added, 1 part of pore-foaming agent, obtains composite solution；
S2. composite solution is uniformly coated on carbon cloth surfaces in 15min, reacts 1h at room temperature, then at 60 DEG C
Lower drying, then alternately rinsed with deionization and acetone, finally obtain anode material.
The pore-foaming agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:0.5.
The initiator is ammonium persulfate/sodium sulfite, ammonium persulfate and sodium sulfite in ammonium persulfate/sodium sulfite
Molal weight ratio is 1:0.3.
Comparative example 2
Comparative example 2 in place of the difference of embodiment 2 with being：S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.3
Part hydrophilic graphene, 5 parts of acrylic monomers, it is 1.5 sulfonic acid solutions that 35 parts of aniline monomers, which are added to dress by 300 parts of pH value,
In reactor, it is 5 DEG C to control temperature of reactor with ice-water bath, with 400r/min rotating speed mechanical agitation, then adds 0.3 part and draws
Agent is sent out, obtains composite solution；
The anode material being prepared using embodiment 1~5 and comparative example 1~2 is anode, using stainless steel and iron silk screen as the moon
Pole, tested after biological stable fuel cell with galvanostatic method, the maximum power density and open circuit electricity of test biology fuel cell
Pressure, test data are as shown in the table.
The difference of comparative example 1 and embodiment 2 is that carbon cloth, graphene and the polyaniline of comparative example 1 are all without hydrophilic place
Reason, understood according to the contrast of the test data of comparative example 1 and embodiment 2, electricity of the hydrophily to biological fuel cell anode material
Performance has a significant effect, and the good anode material of hydrophily has more preferable electricity generation performance；According to comparative example 2 and embodiment 2
Test data contrast understands that the surface area of pore-foaming agent increase anode material is advantageous to strengthen the electricity generation performance of anode material.
Protection scope of the present invention is not limited merely to above-described embodiment, and all technical schemes for belonging under thinking of the present invention are equal
Belong to protection scope of the present invention.It should be pointed out that for those skilled in the art, the present invention is not being departed from
Some improvements and modifications under the premise of principle, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of biological fuel cell anode material, it is characterised in that comprise the following steps：
S1. count in parts by weight, 5 parts of single-layer graphene oxides, 5~8 parts of styrene sulfonic acids and 100 parts of deionized waters mixed,
24h is stirred at room temperature, then adds 5~7 parts of hydrazine hydrates, flow back 8~12h at 90~95 DEG C, then filtration washing, will be solid
Body product vacuum is dried, and obtains hydrophilic graphene；
S2. count in parts by weight, by 5 parts of polystyrolsulfon acids, 0.3~0.9 part of hydrophilic graphene, 1~5 part of acrylic acid list
Body, 30~40 parts of aniline monomers are added in reactor of the dress by the sulfonic acid solutions that 300 parts of pH value are 1~1.5, with ice-water bath control
Temperature of reactor processed is 0~5 DEG C, with 400~500r/min rotating speed mechanical agitation, then adds 0.25~0.3 part of initiator,
1~3 part of pore-foaming agent, obtains composite solution；
S3. composite solution is uniformly coated on carbon cloth surfaces, reacts 1~2h at room temperature, then dried at 55~60 DEG C,
Alternately rinsed with deionization and acetone again, finally obtain anode material.
A kind of 2. preparation method of biological fuel cell anode material according to claim 1, it is characterised in that the carbon
By pre-processing, preprocess method is cloth：Carbon cloth is immersed in ethanol or acetone soln, then 0.5~1h of ultrasonic vibration, so
Take out and dry afterwards, be then placed in the hydrogen peroxide that concentration is 20~30% and soak 6~8h, rinsed and then dried standby with water.
3. the preparation method of a kind of biological fuel cell anode material according to claim 1, it is characterised in that described multiple
Close solution and carbon cloth surfaces are coated in 15min.
A kind of 4. preparation method of biological fuel cell anode material according to claim 1, it is characterised in that the cause
Hole agent is the mixture of sodium carbonate and sodium acid carbonate, and the mass ratio of sodium carbonate and sodium acid carbonate is 1:0.5~1.3.
5. the preparation method of a kind of biological fuel cell anode material according to claim 1, it is characterised in that described to draw
Hair agent is ammonium persulfate, potassium peroxydisulfate, any one in ammonium persulfate/sodium sulfite, over cure in ammonium persulfate/sodium sulfite
The molal weight ratio of sour ammonium and sodium sulfite is 1:0.1~0.3.
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Cited By (2)
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| CN110943230A (en) * | 2019-11-21 | 2020-03-31 | 南京师范大学 | Microbial fuel cell anode and preparation method thereof |
| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
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