CN107973282A - A kind of carbon material and preparation method and application produces hydrogen peroxide in electro-catalysis - Google Patents
A kind of carbon material and preparation method and application produces hydrogen peroxide in electro-catalysis Download PDFInfo
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- CN107973282A CN107973282A CN201711049288.1A CN201711049288A CN107973282A CN 107973282 A CN107973282 A CN 107973282A CN 201711049288 A CN201711049288 A CN 201711049288A CN 107973282 A CN107973282 A CN 107973282A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/28—Per-compounds
- C25B1/30—Peroxides
Abstract
The invention discloses a kind of carbon material and preparation method and application hydrogen peroxide is produced in electro-catalysis.The carbon material is standby by high temperature cabonization walnut kernel leather, is dropped in after which is dispersed in ethanol solution on carbon cloth, is used further to electro-catalysis redox reactions, and reaction product is water（4e‑Approach）：O2+4H++4e‑→2H2O；Or water and hydrogen peroxide（2e‑Approach）：O2+2H++2e‑→H2O2, H2O2+2H++2e‑→2H2O.The material is cheap, renewable, can be mass-produced preparation；With loose structure, the diffusion of oxygen can be promoted；There is micro metallic element, improve the electric conductivity of carbon material to promote the transmission of electronics.In alkaline conditions, when which being used for electro-catalysis redox reactions, there is higher selectivity for the approach of oxygen reduction, specifically, to the 2e of redox reactions‑Approach, which produces hydrogen peroxide intermediate product, higher coulombic efficiency.
Description
Technical field
The invention belongs to electrocatalysis material field, and in particular to a kind of carbon material and preparation method and application is in electro-catalysis
Produce hydrogen peroxide.
Background technology
Hydrogen peroxide (hydrogen peroxide) is not only oxidizing but also has reproducibility and uses rear non-secondary pollution, is defined as green
Chemical products, and it is widely used in the multiple fields such as chemicals synthesis, medical preparation, industrial bleaching, military project, food and environment,
With broad based growth prospect.The most ripe method of industrial large-scale production hydrogen peroxide is anthraquinone at present, but it is anthraquinone not
Only complex steps, can also use some organic solvents so that cause secondary pollution to environment in preparation process, therefore find one
The method production hydrogen peroxide of kind green high-efficient is extremely urgent.
In electrochemical reduction O2Become H2In the reaction of O, there are two kinds of reaction paths, i.e. 4e-Approach：O2+4H++4e-→2H2O
And 2e-Approach O2+2H++2e-→H2O2, H2O2+2H++2e-→2H2O, and the selection of catalyst be determine reaction path it is crucial because
One of element, therefore, selects a kind of suitable catalyst to promote the 2e of redox reactions-Approach, produces and accumulates a large amount of
H2O2, achieve the purpose that small-scale efficient green production hydrogen peroxide.The effective catalyst of electrocatalytic oxidation reduction reaction at present, greatly
Part is all catalysis selection 4e-Approach；A small number of noble metal catalysts can be catalyzed selection 2e-Approach, it is expensive, and will
The crystallinity of accurate control catalyst and crystal face etc., preparation condition is harsh.The performance of carbon material electro-catalysis redox reactions is not
Height, can but promote 2e-The generation of approach, so as to be conducive to generate hydrogen peroxide.
The content of the invention
The shortcomings that in order to solve the prior art and shortcoming, it is an object of the invention to provide a kind of carbon material and its system
Preparation Method with applied to electro-catalysis production hydrogen peroxide, the preparation method is simple, raw material cheap reproducible, is easy to industrialize big rule
Mould produces, and the carbon material being prepared has high selectivity during electro-catalysis reduces oxygen production hydrogen peroxide.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of carbon material, comprises the following steps：
(1) walnut is put into after being soaked in warm water to strip off walnut kernel skin stand-by, then by walnut kernel skin be successively placed on water and
It is ultrasonic in ethanol, place into dry in air dry oven；
(2) by dried walnut kernel skin high-temperature calcination under an argon atmosphere, porous carbon material is obtained.
Preferably, the temperature of warm water described in step (1) is 50~90 DEG C；The ultrasonic time is 3~5h；It is described dry
Dry temperature is 60~80 DEG C.
Preferably, the flow velocity of argon gas described in step (2) is 40~70mL/min.
Preferably, heating rate when being calcined described in step (2) is 2~5 DEG C/min；The temperature of the calcining is 800
~1000 DEG C；The time of the calcining is 4~6h.
A kind of carbon material as made from above-described preparation method, the carbon material have loose structure；Containing trace meter
Element (such as Ca, Mg, Al) and micro nonmetalloid (such as P, S, F)；The carbon material is applied to electro-catalysis production hydrogen peroxide, to oxygen
The 2e of gas reduction reaction-Approach, which produces hydrogen peroxide intermediate product, higher coulombic efficiency.
Preferably, which comprises the following steps：
Carbon material is dispersed in ethanol solution and is dropped on carbon cloth, is used for electro-catalysis oxygen as working electrode after drying
Hydrogen peroxide is prepared in reduction reaction.
It is further preferred that the concentration that the carbon material is dispersed in ethanol solution is 4~8mg/mL.
It is further preferred that the area of the carbon cloth is 1~3cm2；The carbon solution dropped on carbon cloth is 100~400 μ L；
The temperature of the drying is 60~80 DEG C.
It is further preferred that the system for electro-catalysis redox reactions is three-electrode system, wherein carbon material electrode
As working electrode, carbon-point is used as to electrode, and for saturated calomel electrode as reference electrode, electrolyte used in test is 0.1M
KOH solution, test potential are 0~0.9V (relative to standard hydrogen electrode).
Compared with prior art, the present invention has the following advantages and beneficial effect：
(1) present invention prepare carbon material technique it is simple, raw material is cheap and easy to get renewable, can large-scale industrial production.
(2) carbon material of the invention has loose structure, can promote the diffusion of oxygen；There is micro metallic element (such as
Ca, Mg, Al), the electric conductivity of carbon material is improved to promote the transmission of electronics.
(3) carbon material of the invention, which is used for electro-catalysis production hydrogen peroxide, has high selectivity, i.e., to redox reactions
2e-Approach, which produces hydrogen peroxide intermediate product, higher coulombic efficiency.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of carbon material made from embodiment 1；
Fig. 2 is the energy spectrum diagram of carbon material made from embodiment 1；
Fig. 3 is the linear scan curve map that carbon material electrode made from embodiment 1 is used for electro-catalysis redox reactions；
Fig. 4 is the current versus time curve figure that carbon material electrode made from embodiment 1 is used for electro-catalysis redox reactions；
Fig. 5 is that carbon material electrode is used for the canonical plotting that electro-catalysis produces the content of hydrogen peroxide in embodiment 1~3.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
The present embodiment it is a kind of for electro-catalysis production hydrogen peroxide carbon material methods for making and using same, specifically include with
Lower step：
(1) walnut is put into 50 DEG C of water and soaks half an hour, by obtained walnut kernel skin successively in distilled water and ethanol
In each ultrasound 3h, it is then dry under the conditions of 60 DEG C in air dry oven.
(2) the walnut kernel skin that gained is dried is put into tube furnace, under the conditions of argon gas flow velocity 40mL/min, 2 DEG C/min
800 DEG C are warming up to, calcination time 6h.The scanning electron microscope (SEM) photograph of gained carbon material is as shown in Figure 1, it is seen that carbon materials obtained by the present embodiment
Material has loose structure.Fig. 2 be gained carbon material energy spectrum diagram, it is seen that have in gained carbon material minor metallic element (such as Ca,
Mg、Al)。
(3) will be dispersed in after gained carbon materials abrasive lapping in ethanol solution (99wt%), concentration 4mg/mL；Take 400 μ L drops
In 1cm2On carbon cloth, it is then placed in air dry oven under the conditions of 60 DEG C dry.Gained carbon material electrode is as work after drying
Electrode (cathode) is used to prepare hydrogen peroxide in electro-catalysis redox reactions.Electricity is used for carbon material electrode using three-electrode system
The performance that catalytic oxygen reduction reaction prepares hydrogen peroxide is tested, and wherein carbon material electrode is as working electrode, carbon-point conduct
To electrode, for saturated calomel electrode as reference electrode, electrolyte used in test is 0.1M KOH solutions.Fig. 3 is electrochemistry
Linear scanning curve is tested, voltage range is in 0-0.9V, from the figure 3, it may be seen that gained carbon material has the performance that catalytic oxygen reduces.For
The selectivity of further research catalytic oxygen reduction reaction generation hydrogen peroxide, test respectively under different potentials (0.4V,
0.5V, 0.6V, 0.7V, 0.8V) generation hydrogen peroxide efficiency and yield.Fig. 4 is the current versus time curve figure of test, can by Fig. 4
Know under each current potential, current versus time curve is all relatively stablized, and further embodies the stability of gained carbon material.
The content of hydrogen peroxide carries out quantitative analysis according to National Standard Method (GB/T23499-2009), and Fig. 5 measures hydrogen peroxide standard specimen for National Standard Method
Absorbance-concentration standard curve figure, as shown in Figure 5 gained standard curve degree of fitting it is very high, meet the requirements, can be used as mark
Standard uses.The carbon material electrode obtained by the present embodiment of table 1 is used for electro-catalysis production hydrogen peroxide and produces hydrogen peroxide under different potentials
Efficiency and yield.
Table 1
Embodiment 2
The present embodiment it is a kind of for electro-catalysis production hydrogen peroxide carbon material methods for making and using same, specifically include with
Lower step：
(1) walnut is put into 70 DEG C of water and soaks half an hour, by obtained walnut kernel skin successively in distilled water and ethanol
In each ultrasound 4h, it is then dry under the conditions of 70 DEG C in air dry oven.
(2) the walnut kernel skin that gained is dried is put into tube furnace, under the conditions of argon gas flow velocity 50mL/min, 4 DEG C/min
900 DEG C are warming up to, calcination time 5h, obtains carbon material.The scanning electron microscope (SEM) photograph of gained carbon material is similar to Fig. 1, by scanning electron microscope
Figure understands that carbon material obtained by the present embodiment has loose structure.The energy spectrum diagram of gained carbon material is similar to Fig. 2, it is known that the present embodiment
Gained carbon material contains minor metallic element (such as Ca, Mg, Al).
(3) will be dispersed in after gained carbon materials abrasive lapping in ethanol solution (99wt%), concentration 6mg/mL；Take 300 μ L drops
In 2cm2On carbon cloth, it is then placed in air dry oven under the conditions of 70 DEG C dry.Gained carbon material electrode is as work after drying
Electrode (cathode) prepares hydrogen peroxide applied to electro-catalysis oxygen reduction.Electro-catalysis is used for carbon material electrode using three-electrode system
The performance that redox reactions prepare hydrogen peroxide is tested, and wherein carbon material electrode is used as to electricity as working electrode, carbon-point
Pole, for saturated calomel electrode as reference electrode, electrolyte used in test is 0.1M KOH solutions.Wherein, electro-chemical test
The voltage range of linear scan is in 0-0.9V, and it is raw to test under different potentials (0.4V, 0.5V, 0.6V, 0.7V, 0.8V) respectively
Into the efficiency and yield of hydrogen peroxide.The content of hydrogen peroxide carries out quantitative analysis, national standard according to National Standard Method (GB/T 23499-2009)
Method measures absorbance-concentration standard curve figure of hydrogen peroxide standard specimen obtained by the present embodiment with reference to figure 5, it is known that gained standard curve
Degree of fitting is very high, meets the requirements, and can be used as standard.The carbon material electrode obtained by the present embodiment of table 2 is given birth to for electro-catalysis
Production hydrogen peroxide produces the efficiency and yield of hydrogen peroxide under different potentials.
Table 2
Embodiment 3
The present embodiment it is a kind of for electro-catalysis production hydrogen peroxide carbon material methods for making and using same, specifically include with
Lower step：
(1) walnut is put into 80 DEG C of water and soaks half an hour, by obtained walnut kernel skin successively in distilled water and ethanol
In each ultrasound 5h, it is then dry under the conditions of 80 DEG C in air dry oven.
(2) the walnut kernel skin that gained is dried is put into tube furnace, under the conditions of argon gas flow velocity 70mL/min, 5 DEG C/min
1000 DEG C are warming up to, calcination time 4h, obtains carbon material.The scanning electron microscope (SEM) photograph of gained carbon material is similar to Fig. 1, by scanning electron microscope
Figure understands that carbon material obtained by the present embodiment has loose structure.The energy spectrum diagram of gained carbon material is similar to Fig. 2, it is known that the present embodiment
Gained carbon material contains minor metallic element (such as Ca, Mg, Al).
(3) will be dispersed in after gained carbon materials abrasive lapping in ethanol solution (99wt%), concentration 8mg/mL；Take 200 μ L drops
In 2cm2On carbon cloth, it is then placed in air dry oven under the conditions of 70 DEG C dry.Gained carbon material electrode is as work after drying
Electrode (cathode) is used to prepare hydrogen peroxide in electro-catalysis redox reactions.Electricity is used for carbon material electrode using three-electrode system
The performance that catalytic oxygen reduction reaction prepares hydrogen peroxide is tested, and wherein carbon material electrode is as working electrode, carbon-point conduct
To electrode, for saturated calomel electrode as reference electrode, electrolyte used in test is 0.1M KOH solutions.Wherein, electrochemistry
Test linear scan voltage range in 0-0.9V, and test respectively under different potentials (0.4V, 0.5V, 0.6V, 0.7V,
0.8V) generate the efficiency and yield of hydrogen peroxide.The content of hydrogen peroxide is quantitatively divided according to National Standard Method (GB/T 23499-2009)
Analysis, National Standard Method measure absorbance-concentration standard curve figure of hydrogen peroxide standard specimen obtained by the present embodiment with reference to figure 5, it is known that gained mark
The degree of fitting of directrix curve is very high, meets the requirements, and can be used as standard.The carbon material electrode obtained by the present embodiment of table 3 is used for
Electro-catalysis production hydrogen peroxide produces the efficiency and yield of hydrogen peroxide under different potentials.
Table 3
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of carbon material, it is characterised in that comprise the following steps：
（1）Walnut is put into after being soaked in warm water to strip off walnut kernel skin stand-by, walnut kernel skin is then successively placed on water and ethanol
Middle ultrasound, places into dry in air dry oven；
（2）By dried walnut kernel skin high-temperature calcination under an argon atmosphere, porous carbon material is obtained.
2. preparation method according to claim 1, it is characterised in that step（1）Described in warm water temperature be 50 ~ 90
℃；The ultrasonic time is 3 ~ 5h；The temperature of the drying is 60 ~ 80 DEG C.
3. preparation method according to claim 1, it is characterised in that step（2）Described in argon gas flow velocity for 40 ~
70mL/min。
4. preparation method according to claim 1, it is characterised in that step（2）Described in calcine when heating rate be 2
~5℃/min；The temperature of the calcining is 800 ~ 1000 DEG C；The time of the calcining is 4 ~ 6h.
A kind of 5. carbon material as made from claim 1 ~ 4 any one of them preparation method.
6. a kind of carbon material described in claim 5 is applied to electro-catalysis production hydrogen peroxide.
7. application according to claim 6, it is characterised in that comprise the following steps：
Carbon material is dispersed in ethanol solution and is dropped on carbon cloth, is used for electro-catalysis oxygen reduction as working electrode after drying
Hydrogen peroxide is prepared in reaction.
8. application according to claim 7, it is characterised in that the carbon material be dispersed in concentration in ethanol solution for 4 ~
8mg/mL。
9. application according to claim 7, it is characterised in that the area of the carbon cloth is 1 ~ 3cm2；Drop in the carbon on carbon cloth
Solution is 100 ~ 400 μ L；The temperature of the drying is 60 ~ 80 DEG C.
10. application according to claim 7, it is characterised in that the electrolyte for electro-catalysis redox reactions is
0.1M KOH solutions, test potential are 0 ~ 0.9V.
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| CN109622014A (en) * | 2018-12-12 | 2019-04-16 | 安徽大学 | A kind of preparation method of the catalyst of electro-catalysis oxygen generation hydrogen peroxide |
| CN109941995A (en) * | 2019-04-04 | 2019-06-28 | 济南大学 | A kind of preparation and application of the heteroatom doping biomass carbon material producing hydrogen peroxide for electro-catalysis |
| CN110528019A (en) * | 2019-09-05 | 2019-12-03 | 大连理工大学 | A kind of portable domestic production H2O2Solution containment and method |
| CN111962099A (en) * | 2020-08-20 | 2020-11-20 | 中国科学院宁波材料技术与工程研究所 | Electrode for electrocatalytic production of hydrogen peroxide, preparation method and application thereof |
| CN112725822A (en) * | 2020-12-15 | 2021-04-30 | 济南大学 | Oxidation method of carbon nano tube and application thereof |
| CN113481004A (en) * | 2021-05-21 | 2021-10-08 | 浙江工业大学 | Carbon dots and preparation method and application thereof |
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| CN114703504A (en) * | 2022-03-22 | 2022-07-05 | 华南理工大学 | Transition metal-loaded carbon fiber catalyst, preparation thereof and application thereof in electrocatalytic synthesis of hydrogen peroxide |
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