CN108866569A - A kind of preparation method of teflon heat modification gas-diffusion electrode - Google Patents
A kind of preparation method of teflon heat modification gas-diffusion electrode Download PDFInfo
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- CN108866569A CN108866569A CN201810714955.1A CN201810714955A CN108866569A CN 108866569 A CN108866569 A CN 108866569A CN 201810714955 A CN201810714955 A CN 201810714955A CN 108866569 A CN108866569 A CN 108866569A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/042—Electrodes formed of a single material
- C25B11/043—Carbon, e.g. diamond or graphene
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C—CHEMISTRY; METALLURGY
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
Abstract
The invention belongs to electrochemical technology fields, it is related to a kind of preparation method of teflon heat modification gas-diffusion electrode, conductive black, dehydrated alcohol are mixed with ptfe emulsion first, obtained mix products are heat-treated to get conductive black/PTFE composite；Then it is mixed again using obtained composite material as presoma with dehydrated alcohol, ptfe emulsion, obtain mixed emulsion, mixed emulsion is rolled on stainless (steel) wire, obtain preliminary gas-diffusion electrode, it is calcined in Muffle furnace again to get teflon heat modification gas-diffusion electrode.Present invention improves over the synthesis technologies of traditional gas diffusion electrode, by PTFE while as adhesive, the modifying agent effect for also playing conductive black catalyst, so that the gas-diffusion electrode catalytic activity with higher and stability that are synthesized by two step high-temperature technologies.
Description
Technical field
The invention belongs to electrochemical technology fields, are related to a kind of system of teflon heat modification gas-diffusion electrode
Preparation Method.
Background technique
In recent years, gas-diffusion electrode is used for electro-catalysis and produces H2O2Field, which is repaired, in water pollution causes extensive concern,
In the O of gas-diffusion electrode surface enrichment in the reaction process2H can be converted by two electronic reduction reactions2O2.Electrochemistry is former
The H that position generates2O2It can be converted into the hydroxyl radical free radical with strong oxidizing property by ultraviolet excitation and Fenton's reaction, thus real
The efficient degradation removing of pollutant in existing water body.
Gas-diffusion electrode is the electrode of an electrochemical reaction for having solid, liquid, gas phase reaction, therefore gas diffusion is electric
It extremely mainly include gas diffusion layers (gas diffusion layer), Catalytic Layer (catalyst layer) collector
(current collector) three parts.Gas diffusion layers play the role of waterproof and conveying gas；Catalytic Layer is responsible for providing three-phase
Reaction zone；Collector then plays electric current and collects and transmit.Currently, carbon black/polytetrafluoroethylene (PTFE) (PTFE) combination electrode is to grind
Study carefully most commonly used gas-diffusion electrode, main preparation process is to mix carbon black, PTFE and ethyl alcohol, dry, and is then passed through
Cross roll and a step high-temperature heat treatment process synthesis.The resulting gas-diffusion electrode of the preparation process has the following problems：
(1) electrode catalyst activity is to be improved
In gas-diffusion electrode active sites, the reduction of oxygen is in addition to two electron reductions generation H2O2Outside, four electricity can also be passed through
Sub- reaction path generates H2The potential window intermeshing of O, two electronics and four electronics.The characteristic makes electrode in high current density
Under the conditions of polarity effect is significant when working, and then reduce electrolytically generated H2O2Current efficiency, increase energy consumption.
(2) electrode catalyst active sites stability is poor
The catalytic activity that carbon black-PTFE gas-diffusion electrode preparation process defect itself causes it to be difficult to have more stable.
PTFE can occur to peel off after high-temperature process, shrink, so that carbon black catalytic active site is exposed in electrode surface.Therefore, electrode
After long-play, chemical attack easily occurs material for exposed catalyst in the solution.
Summary of the invention
According to the above-mentioned deficiencies of the prior art, in order to promote carbon black/PTFE gas-diffusion electrode catalytic activity and stabilization
Property, the present invention proposes a kind of preparation method of teflon heat modification gas-diffusion electrode, the main feature of this method
It is to be compared to one-step method heat containing high-temperature heat treatment process and low temperature heat-treatment process in the synthesis technology of gas-diffusion electrode
For the conventional carbon black/PTFE electrode for handling synthesis, the electrode of this patent synthesis has higher H2O2Yield and stability.
The specific technical solution of the present invention is as follows：A kind of preparation side of teflon heat modification gas-diffusion electrode
Method, it is characterised in that include the following steps：
Step 1 mixes conductive black, dehydrated alcohol with ptfe emulsion, by obtained mix products into
Row heat treatment is to get conductive black/PTFE composite；
Step 2, the composite material that step 1 is obtained as presoma and dehydrated alcohol, ptfe emulsion again
Mixing, obtains mixed emulsion, mixed emulsion is rolled on stainless (steel) wire, obtain preliminary gas-diffusion electrode, then by it in horse
Not calcine in furnace to get teflon heat modification gas-diffusion electrode.
Wherein preferred embodiment is as follows：
The model VXC-72 of the conductive black, VXC-72R, Printex L6 or Printex25.
The mass fraction of the ptfe emulsion is 30%~60%.
In the step one, the mixed proportion of conductive black, dehydrated alcohol and ptfe emulsion is 1~3g：50
~120mL：0~10mL.
In the step one, the temperature that mix products are heat-treated is 400~1200 DEG C, and the time is 0.5~2h.
In the step two, the mixed proportion of composite material, dehydrated alcohol and ptfe emulsion is 0.5~2g：
50~120mL：5~10mL.
In the step two, the mesh number of stainless (steel) wire is 40~80 mesh, and the pressure for rolling compacting is 10~20MPa, just
Walk gas-diffusion electrode with a thickness of 0.5~2mm.
In the step two, the calcination temperature in Muffle furnace is 200~400 DEG C, and the time is 0.5~2h.
The principle of the present invention is：Heat modification processing is carried out to the mixed liquor of conductive black, dehydrated alcohol and PTFE first, it is high
PTFE is cracked under temperature effect, closes C-C bond in wherein fluorine-containing functional group and conductive black, thus on conductive black surface
Fluorine-containing functional group is generated, the network structure to interweave can be formed, while also can guarantee that good gas transport and enough ions are logical
Road, makes electrode have better catalytic effect, and the catalysis of lift gas diffusion electrode generates H2O2Efficiency.In addition, compared to tradition
Direct mixing, drying, roll-in synthesis electrode, electrode prepared by this method has more preferably electric conductivity and stronger hydrophobic
Performance.Therefore, the technology for preparing electrode being related in the present invention has important meaning for the industrial applications of gas-diffusion electrode
Justice.
Compared with prior art, the beneficial effects of the present invention are：The synthesis technology of traditional gas diffusion electrode is improved,
By PTFE while as adhesive, the modifying agent effect of conductive black catalyst is also played.By first step high temperature
PTFE contains more fluorine-containing functional group in modified conductive black surface, which can not only increase having for carbon blacksurface
Catalytic active site is imitated, while improving the hydrophobic performance of conductive black material, so that by the synthesis of two step high-temperature technologies
Gas-diffusion electrode catalytic activity with higher and stability.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, to the technology in the embodiment of the present invention
Scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1：
A kind of preparation method of teflon heat modification gas-diffusion electrode, includes the following steps：
Step 1：The conductive black for weighing 1g is dissolved in the dehydrated alcohol of 80mL, and 5mL PTFE is added after mixing,
Ultrasonic disperse is uniform, obtains mixed emulsion.Mixed emulsion is stirred continuously at 80 DEG C, obtains paste after ethyl alcohol volatilization.
By paste in 90 DEG C of drying 2h, it is subsequently placed in tube furnace in 500 DEG C of high-temperature calcination 1h, it is multiple obtains novel conductive carbon black/PTFE
Condensation material.
Step 2：Novel conductive carbon black/PTFE composite is rolled into powder and weighs 0.5g novel conductive carbon black/PTFE powder
End is mixed in the ethanol solution of 100mL, and the ptfe emulsion of 7mL is added after mixing, and ultrasonic disperse is equal
It is even, obtain mixed emulsion.Mixed emulsion is stirred continuously at 80 DEG C, obtains paste after ethyl alcohol volatilization, paste is equal
It is pressed on the stainless (steel) wire for 60 mesh got ready in advance evenly, the pressure modulation 15MPa on roller is pressed into the piece of 2mm.It will
The pellet electrode being pressed into is placed in Muffle furnace to be calcined in 320 DEG C, obtains novel gas diffusion electrodes.
Using this electrode as cathode in the preparation of yields of hydrogen peroxide, reaction carry out 120min after, hydrogen peroxide
Yield is up to 131.4mg/L.
Embodiment 2：
The preparation method of teflon heat modification gas-diffusion electrode as described in Example 1, unlike：
In step 1, the dosage of PTFE is 7mL, and it is 900 DEG C that required temperature is calcined in tube furnace.
Using this electrode as cathode in the preparation of yields of hydrogen peroxide, reaction carry out 120min after, hydrogen peroxide
Yield is up to 153.7mg/L.
Embodiment 3：
The preparation method of teflon heat modification gas-diffusion electrode as described in Example 1, unlike：
In step 1, the dosage of PTFE is 9mL, and it is 1200 DEG C that required temperature is calcined in tube furnace.
Using this electrode as cathode in the preparation of yields of hydrogen peroxide, reaction carry out 120min after, hydrogen peroxide
Yield is up to 121.3mg/L.
Comparison example 1：
The preparation method of teflon heat modification gas-diffusion electrode as described in Example 1, unlike：
In step 1, the dosage of PTFE is 0mL, and it is 900 DEG C that required temperature is calcined in tube furnace.
Using this electrode as cathode in the preparation of yields of hydrogen peroxide, reaction carry out 120min after, hydrogen peroxide
Yield is 71.1mg/L.
Comparison example 2：
The preparation method of teflon heat modification gas-diffusion electrode as described in Example 1, unlike：
Directly with unmodified conductive black material, gas-diffusion electrode only is made according to the method for step 2.
Using this electrode as cathode in the preparation of yields of hydrogen peroxide, reaction carry out 120min after, hydrogen peroxide
Yield is 82.9mg/L.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (8)
1. a kind of preparation method of teflon heat modification gas-diffusion electrode, it is characterised in that include the following steps：
Step 1 mixes conductive black, dehydrated alcohol with ptfe emulsion, and obtained mix products are carried out heat
Processing is to get conductive black/PTFE composite；
Step 2 mixes the composite material that step 1 obtains as presoma with dehydrated alcohol, ptfe emulsion again,
Mixed emulsion is obtained, mixed emulsion is rolled on stainless (steel) wire, obtains preliminary gas-diffusion electrode, then by it in Muffle furnace
Calcining is to get teflon heat modification gas-diffusion electrode.
2. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：The model VXC-72 of the conductive black, VXC-72R, Printex L6 or Printex25.
3. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：The mass fraction of the ptfe emulsion is 30%~60%.
4. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：In the step one, the mixed proportion of conductive black, dehydrated alcohol and ptfe emulsion is 1~3g：50~
120mL：0~10mL.
5. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：In the step one, the temperature that mix products are heat-treated is 400~1200 DEG C, and the time is 0.5~2h.
6. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：In the step two, the mixed proportion of composite material, dehydrated alcohol and ptfe emulsion is 0.5~2g：50
~120mL：5~10mL.
7. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：In the step two, the mesh number of stainless (steel) wire is 40~80 mesh, and the pressure for rolling compacting is 10~20MPa, tentatively
Gas-diffusion electrode with a thickness of 0.5~2mm.
8. a kind of preparation method of teflon heat modification gas-diffusion electrode according to claim 1, special
Sign is：In the step two, the calcination temperature in Muffle furnace is 200~400 DEG C, and the time is 0.5~2h.
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| CN201810714955.1A CN108866569B (en) | 2018-07-03 | 2018-07-03 | Preparation method of novel polytetrafluoroethylene thermal modification gas diffusion electrode |
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| CN201810714955.1A CN108866569B (en) | 2018-07-03 | 2018-07-03 | Preparation method of novel polytetrafluoroethylene thermal modification gas diffusion electrode |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110565112A (en) * | 2019-08-19 | 2019-12-13 | 天津大学 | method for changing cathode oxygen reduction activity by regulating hydrophilicity and hydrophobicity |
| CN110965077A (en) * | 2019-12-04 | 2020-04-07 | 武汉科技大学 | Preparation method of single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide |
| CN112875811A (en) * | 2021-01-19 | 2021-06-01 | 南京工业大学 | Method for preparing electrocatalytic gas diffusion electrode by using waste tires |
| CN113439132A (en) * | 2019-02-15 | 2021-09-24 | 阿凡田知识中心有限公司 | Method for producing a gas diffusion layer and gas diffusion layer obtained or obtainable by said method |
| CN113718280A (en) * | 2021-08-31 | 2021-11-30 | 苏州清缘环保科技有限公司 | Gas diffusion electrode and method for producing same |
| CN114774959A (en) * | 2022-04-25 | 2022-07-22 | 中国科学院城市环境研究所 | Integrated carbon electrode for producing hydrogen peroxide by air diffusion device and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113439132A (en) * | 2019-02-15 | 2021-09-24 | 阿凡田知识中心有限公司 | Method for producing a gas diffusion layer and gas diffusion layer obtained or obtainable by said method |
| CN110565112A (en) * | 2019-08-19 | 2019-12-13 | 天津大学 | method for changing cathode oxygen reduction activity by regulating hydrophilicity and hydrophobicity |
| CN110965077A (en) * | 2019-12-04 | 2020-04-07 | 武汉科技大学 | Preparation method of single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide |
| CN112875811A (en) * | 2021-01-19 | 2021-06-01 | 南京工业大学 | Method for preparing electrocatalytic gas diffusion electrode by using waste tires |
| CN112875811B (en) * | 2021-01-19 | 2022-08-05 | 南京工业大学 | Method for preparing electrocatalytic gas diffusion electrode by using waste tires |
| CN113718280A (en) * | 2021-08-31 | 2021-11-30 | 苏州清缘环保科技有限公司 | Gas diffusion electrode and method for producing same |
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| CN114774959A (en) * | 2022-04-25 | 2022-07-22 | 中国科学院城市环境研究所 | Integrated carbon electrode for producing hydrogen peroxide by air diffusion device and preparation method and application thereof |
| CN114774959B (en) * | 2022-04-25 | 2024-02-20 | 中国科学院城市环境研究所 | Integrated carbon electrode for producing hydrogen peroxide by air diffusion device and preparation method and application thereof |
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