CN107732255A - A kind of combination electrode of graphene-containing and metal organic frame and preparation method thereof - Google Patents
A kind of combination electrode of graphene-containing and metal organic frame and preparation method thereof Download PDFInfo
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- CN107732255A CN107732255A CN201710793696.1A CN201710793696A CN107732255A CN 107732255 A CN107732255 A CN 107732255A CN 201710793696 A CN201710793696 A CN 201710793696A CN 107732255 A CN107732255 A CN 107732255A
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Abstract
The invention discloses combination electrode of a kind of graphene-containing and metal organic frame and preparation method thereof, the preparation method of the combination electrode comprises the following steps：1) pre-treatment of graphite cake；2) anodic oxidation stripping prepares graphene；3) modification of graphene；4) preparation of metal organic frame.The graphene-containing of the present invention and the combination electrode of metal organic frame have the advantages that specific surface area is big, resistance is low, Stability Analysis of Structures, the advantages of not only taking full advantage of graphene and big metal organic frame specific surface area, also overcome the shortcomings that metal organic frame electric conductivity is bad simultaneously, both advantages are given full play of, the electrode may be used as the anode of bioelectrochemical system.
Description
Technical field
The present invention relates to combination electrode of a kind of graphene-containing and metal organic frame and preparation method thereof.
Background technology
Bioelectrochemical system (Bio-electrochemical system, BES) is that one kind can carry out waste water simultaneously
Processing and the new device of electrical energy production, in recovery (such as microorganism production of pollutant in-situ immobilization, sewage disposal and biomass energy
Power technology) etc. show good application prospect.However, BES has the defects of power output is not high at present, it is limited
Application in production.It is that to carry BES defeated that electrode, which is modified, or increases the method for electrode surface area using three-diemsnional electrode etc.
Go out the main path of power.
Because graphene has the advantages that specific surface area is big, electrical and thermal conductivity performance is excellent, the decorative material of anode is commonly used for.
Research shows, the overall performance that can significantly improve BES is modified electrode using graphene, but because graphene is usually
Bonded by adhesive and electrode material, not only less stable, and contact resistance is also higher, and the performance of graphene is excellent
Gesture can not greatly be brought into play.In order to eliminate power consumption caused by contact resistance, it is system to be formed in situ graphene
One fine method of standby BES anodes.For example, Yong Yangchun etc. is had found by studying, electroactive microorganism Shewanella
Oneidensis MR-1 can in-situ reducing graphene oxide, when in this, as MFC anodes, 843 ± 31mW/m can be obtained2
Power density, be 22 times of the anode without graphene modified.However, process of the existing technique in production graphene oxide
It is middle to need using the reagent with larger toxicity, and production process can also produce poisonous and hazardous accessory substance, can bring serious
Environmental pollution.
Metal organic frame (MOFs) material is made up of the combination of organic bridge ligand and inorganic metal ion
Ordered network structure.Being compared with existing material, MOFs shows current highest specific surface area and minimum crystalline density, and
Also there is adjustable hole size and functional structure.Therefore, it can be used for the modification of electrode material.However, due to conventional method
The MOFs electrical conductivity of preparation is not high, limits it and is used for BES anode material.
The content of the invention
It is an object of the invention to provide combination electrode of a kind of graphene-containing and metal organic frame and preparation method thereof.
The technical solution used in the present invention is：
A kind of preparation method of the combination electrode of graphene-containing and metal organic frame, comprises the following steps：
1) pre-treatment of graphite cake：Pickling, caustic dip, washing are carried out to graphite cake；
2) anodic oxidation stripping prepares graphene：Two pieces of graphite cakes are taken respectively as negative electrode and anode, in ammonium sulfate
In be electrolysed, anode obtains the graphite cake of surface graphene-containing；
3) modification of graphene：The graphite cake of surface graphene-containing is immersed in NaOH and the chloroacetic aqueous solution, fully
Reaction, obtains graphite cake of the surface containing carboxy-modified graphene；
4) preparation of metal organic frame：Graphite cake of the surface containing carboxy-modified graphene is immersed into ferric nitrate and to benzene two
In the DMF solution of formic acid, fully reaction, the combination electrode of graphene-containing and metal organic frame is obtained.
Pickling described in step 1) is carried out in 0.8~1.2mol/L hydrochloric acid solution, and soak time is 10~20 minutes.
Caustic dip described in step 1) is carried out in 0.8~1.2mol/L NaOH solution, and soak time is 1~1.5 hour.
The molar concentration of ammonium sulfate described in step 2) is 0.8~1.2mol/L.
Electrolysis described in step 2) is carried out under 10~15V of voltage, and electrolysis time is 10~30 minutes.
NaOH, monoxone, the mass ratio of water are 1 in NaOH and the chloroacetic aqueous solution described in step 3)：(0.5~
1.5)：(15~25).
Reaction described in step 3) is carried out under ultrasound, and the reaction time is 2~4 hours.
Ferric nitrate described in step 4) and in the DMF solution of terephthalic acid (TPA) ferric nitrate, terephthalic acid (TPA), DMF quality
Than for 1：(0.3~0.4)：(750~800).
Reaction described in step 4) is carried out at 160~200 DEG C, and the reaction time is 20~30 hours.
The beneficial effects of the invention are as follows：The graphene-containing of the present invention and the combination electrode of metal organic frame have than surface
The advantages that product is big, resistance is low, Stability Analysis of Structures, not only take full advantage of graphene and big excellent of metal organic frame specific surface area
Point, while the shortcomings that metal organic frame electric conductivity is bad is also overcomed, both advantages are given full play of, the electrode can
For use as the anode of bioelectrochemical system.
1) present invention is formed in situ graphene-structured in graphite surface, it is not necessary to adhesive, is not in contact with resistance, stability
It is good；
2) present invention is by graphenic surface carboxyl grafting, then situ Particles shape metal organic frame, and existing
Mixing bonding method compare, it is not in contact with resistance, good conductivity；
3) what the present invention used is all nontoxic or hypotoxicity raw material, and the pollution to environment is small, and will not produce
The harmful intermediate product of poison.
Brief description of the drawings
Fig. 1 is the SEM figures of the graphite cake in embodiment 1.
Fig. 2 is the SEM figures of the graphite cake of the surface graphene-containing in embodiment 1.
Fig. 3 is the SEM figures of the combination electrode of the graphene-containing and metal organic frame in embodiment 1.
Fig. 4 is the XRD of the combination electrode of the graphene-containing and metal organic frame in embodiment 1.
Fig. 5 is the power density test chart of the combination electrode of the graphene-containing and metal organic frame in embodiment 1.
Embodiment
A kind of preparation method of the combination electrode of graphene-containing and metal organic frame, comprises the following steps：
1) pre-treatment of graphite cake：Pickling, caustic dip, washing are carried out to graphite cake；
2) anodic oxidation stripping prepares graphene：Two pieces of graphite cakes are taken respectively as negative electrode and anode, in ammonium sulfate
In be electrolysed, anode obtains the graphite cake of surface graphene-containing；
3) modification of graphene：The graphite cake of surface graphene-containing is immersed in NaOH and the chloroacetic aqueous solution, fully
Reaction, obtains graphite cake of the surface containing carboxy-modified graphene；
4) preparation of metal organic frame：Graphite cake of the surface containing carboxy-modified graphene is immersed into ferric nitrate and to benzene two
In the DMF solution of formic acid, fully reaction, the combination electrode of graphene-containing and metal organic frame is obtained.
Preferably, the pickling described in step 1) is carried out in 0.8~1.2mol/L hydrochloric acid solution, soak time be 10~
20 minutes.
Preferably, the caustic dip described in step 1) is carried out in 0.8~1.2mol/L NaOH solution, soak time be 1~
1.5 hour.
Preferably, the molar concentration of the ammonium sulfate described in step 2) is 0.8~1.2mol/L.
Preferably, the electrolysis described in step 2) is carried out under 10~15V of voltage, and electrolysis time is 10~30 minutes.
Preferably, NaOH, monoxone, the mass ratio of water are 1 in the NaOH described in step 3) and the chloroacetic aqueous solution：
(0.5~1.5)：(15~25).
Preferably, the reaction described in step 3) is carried out under ultrasound, and the reaction time is 2~4 hours.
Preferably, ferric nitrate, terephthalic acid (TPA), DMF in the DMF solution of the ferric nitrate described in step 4) and terephthalic acid (TPA)
Mass ratio be 1：(0.3~0.4)：(750~800).
Preferably, the reaction described in step 4) is carried out at 160~200 DEG C, and the reaction time is 20~30 hours.
The present invention is made further explanation and description with reference to specific embodiment.
Embodiment 1：
A kind of preparation method of the combination electrode of graphene-containing and metal organic frame, comprises the following steps：
1) pre-treatment of graphite cake：It is that 1cm × 2cm × 0.5cm graphite cakes soak in 1mol/L HCl solution by specification
10min, cleaned 3 times with deionized water, then 1h is soaked in 1mol/L NaOH solution, cleaned 3 times with deionized water；
2) anodic oxidation stripping prepares graphene：Two pieces of graphite cakes are taken respectively as negative electrode and anode, apply 12V direct current
Electricity, it is electrolysed in 1mol/L ammonium sulfate, is electrolysed 20min, anode obtains the graphite cake of surface graphene-containing；
3) modification of graphene：The graphite cake of surface graphene-containing is immersed into NaOH and the chloroacetic aqueous solution (NaOH, chlorine
Acetic acid, the mass ratio of water are 1:0.8:20) in, ultrasonic 3h, graphite cake of the surface containing carboxy-modified graphene is obtained；
4) preparation of metal organic frame：Graphite cake of the surface containing carboxy-modified graphene is immersed into ferric nitrate and to benzene two
(ferric nitrate, terephthalic acid (TPA), DMF mass ratio are 1 to the DMF solution of formic acid:0.35:780) in, 180 DEG C of reaction 24h, take out
Graphite cake, with DMF solution wash 3 times, methanol clean 3 times, vacuum freeze drying, obtain answering for graphene-containing and metal organic frame
Composite electrode.
The SEM figures of graphite cake in embodiment 1 are as shown in figure 1, the SEM of the graphite cake of surface graphene-containing is schemed such as Fig. 2 institutes
Show, the SEM of the combination electrode of graphene-containing and metal organic frame figure is as shown in figure 3, graphene-containing and metal organic frame
The XRD of combination electrode is as shown in figure 4, the power density test chart such as figure of the combination electrode of graphene-containing and metal organic frame
Shown in 5.
As shown in Figure 1：The surface of graphite cake is smooth.
As shown in Figure 2：Graphite cake surface after electrolysis forms lamellar graphite alkene structure.
As shown in Figure 3：The graphene layer surface in situ of graphite cake generates granular metal-organic framework.
As shown in Figure 4：Prepared metal organic frame is typical MIL 101-Fe structures.
As shown in Figure 5：After graphene and metal organic frame modification, power density significantly carries graphite plate electrode
Height, maximum power density reach 1.18W/m2, be common graphite plate electrode 2.3 times of (0.508W/m2)。
Embodiment 2：
A kind of preparation method of the combination electrode of graphene-containing and metal organic frame, comprises the following steps：
1) pre-treatment of graphite cake：It is that 1cm × 2cm × 0.5cm graphite cakes soak in 0.8mol/L HCl solution by specification
20min is steeped, is cleaned 2 times with deionized water, then 1h is soaked in 1.2mol/L NaOH solution, is cleaned 3 times with deionized water；
2) anodic oxidation stripping prepares graphene：Two pieces of graphite cakes are taken respectively as negative electrode and anode, apply 15V direct current
Electricity, it is electrolysed in 1mol/L ammonium sulfate, is electrolysed 10min, anode obtains the graphite cake of surface graphene-containing；
3) modification of graphene：The graphite cake of surface graphene-containing is immersed into NaOH and the chloroacetic aqueous solution (NaOH, chlorine
Acetic acid, the mass ratio of water are 1:0.5:25) in, ultrasonic 4h, graphite cake of the surface containing carboxy-modified graphene is obtained；
4) preparation of metal organic frame：Graphite cake of the surface containing carboxy-modified graphene is immersed into ferric nitrate and to benzene two
(ferric nitrate, terephthalic acid (TPA), DMF mass ratio are 1 to the DMF solution of formic acid:0.3:750) in, 200 DEG C of reaction 20h, stone is taken out
Black plate, with DMF solution wash 3 times, methanol clean 2 times, vacuum freeze drying, obtain the compound of graphene-containing and metal organic frame
Electrode.
Embodiment 3：
A kind of preparation method of the combination electrode of graphene-containing and metal organic frame, comprises the following steps：
1) pre-treatment of graphite cake：It is that 1cm × 2cm × 0.5cm graphite cakes soak in 1.2mol/L HCl solution by specification
15min is steeped, is cleaned 3 times with deionized water, then 1.5h is soaked in 0.8mol/L NaOH solution, is cleaned 3 times with deionized water；
2) anodic oxidation stripping prepares graphene：Two pieces of graphite cakes are taken respectively as negative electrode and anode, apply 10V direct current
Electricity, it is electrolysed in 1.2mol/L ammonium sulfate, is electrolysed 30min, anode obtains the graphite cake of surface graphene-containing；
3) modification of graphene：The graphite cake of surface graphene-containing is immersed into NaOH and the chloroacetic aqueous solution (NaOH, chlorine
Acetic acid, the mass ratio of water are 1:1.5:15) in, ultrasonic 2h, graphite cake of the surface containing carboxy-modified graphene is obtained；
4) preparation of metal organic frame：Graphite cake of the surface containing carboxy-modified graphene is immersed into ferric nitrate and to benzene two
(ferric nitrate, terephthalic acid (TPA), DMF mass ratio are 1 to the DMF solution of formic acid:0.4:800) in, 160 DEG C of reaction 30h, stone is taken out
Black plate, with DMF solution wash 3 times, methanol clean 3 times, vacuum freeze drying, obtain the compound of graphene-containing and metal organic frame
Electrode.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by 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)
- A kind of 1. preparation method of the combination electrode of graphene-containing and metal organic frame, it is characterised in that：Comprise the following steps：1) pre-treatment of graphite cake：Pickling, caustic dip, washing are carried out to graphite cake；2) anodic oxidation stripping prepares graphene：Two pieces of graphite cakes are taken to enter respectively as negative electrode and anode in ammonium sulfate Row electrolysis, anode obtain the graphite cake of surface graphene-containing；3) modification of graphene：The graphite cake of surface graphene-containing is immersed in NaOH and the chloroacetic aqueous solution, fully reaction, Obtain graphite cake of the surface containing carboxy-modified graphene；4) preparation of metal organic frame：Graphite cake of the surface containing carboxy-modified graphene is immersed into ferric nitrate and terephthalic acid (TPA) DMF solution in, fully reaction, obtain the combination electrode of graphene-containing and metal organic frame.
- 2. preparation method according to claim 1, it is characterised in that：Pickling described in step 1) is in 0.8~1.2mol/L Hydrochloric acid solution in carry out, soak time be 10~20 minutes.
- 3. preparation method according to claim 1, it is characterised in that：Caustic dip described in step 1) is in 0.8~1.2mol/L NaOH solution in carry out, soak time be 1~1.5 hour.
- 4. preparation method according to claim 1, it is characterised in that：The molar concentration of ammonium sulfate described in step 2) For 0.8~1.2mol/L.
- 5. preparation method according to claim 1, it is characterised in that：Electrolysis described in step 2) is under 10~15V of voltage Carry out, electrolysis time is 10~30 minutes.
- 6. preparation method according to claim 1, it is characterised in that：NaOH and the chloroacetic aqueous solution described in step 3) Middle NaOH, monoxone, the mass ratio of water are 1：(0.5~1.5)：(15~25).
- 7. preparation method according to claim 1, it is characterised in that：Reaction described in step 3) is carried out under ultrasound, instead It is 2~4 hours between seasonable.
- 8. preparation method according to claim 1, it is characterised in that：Ferric nitrate and terephthalic acid (TPA) described in step 4) Ferric nitrate, terephthalic acid (TPA), DMF mass ratio are 1 in DMF solution：(0.3~0.4)：(750~800).
- 9. preparation method according to claim 1, it is characterised in that：Reaction described in step 4) is entered at 160~200 DEG C OK, the reaction time is 20~30 hours.
- 10. graphene-containing and the compound electric of metal organic frame prepared by the method in claim 1~9 described in any one Pole.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982622A (en) * | 2018-04-23 | 2018-12-11 | 中山大学 | Electrochemical sensor and preparation method thereof based on the vertical graphene composite structure of metal organic frame- |
| CN110586041A (en) * | 2019-09-19 | 2019-12-20 | 山东省分析测试中心 | Perfluoroalkyl compound extraction and analysis method based on MOFs stripping graphite phase nitrogen carbide adsorbent |
| CN111318305A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院大连化学物理研究所 | Non-noble metal bifunctional catalyst and preparation method and application thereof |
| CN111333855A (en) * | 2020-04-03 | 2020-06-26 | 华南师范大学 | 1, 5-dihydroxy anthraquinone copper coordination polymer/graphene compound and preparation and application thereof |
| CN112578110A (en) * | 2020-12-16 | 2021-03-30 | 西北农林科技大学 | Biological probe and kit for detecting furacilin and furazolidone and application |
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| CN111333855A (en) * | 2020-04-03 | 2020-06-26 | 华南师范大学 | 1, 5-dihydroxy anthraquinone copper coordination polymer/graphene compound and preparation and application thereof |
| CN112578110A (en) * | 2020-12-16 | 2021-03-30 | 西北农林科技大学 | Biological probe and kit for detecting furacilin and furazolidone and application |
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