CN107055701A - A kind of Fe (Co) SnO2The preparation method of combination electrode - Google Patents

A kind of Fe (Co) SnO2The preparation method of combination electrode Download PDF

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CN107055701A
CN107055701A CN201710376231.6A CN201710376231A CN107055701A CN 107055701 A CN107055701 A CN 107055701A CN 201710376231 A CN201710376231 A CN 201710376231A CN 107055701 A CN107055701 A CN 107055701A
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sno
preparation
electrode
fiber
stannic chloride
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贾哲华
陶翠
赵有华
贾成浩
徐继任
董斌
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Yangzhou University
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Yangzhou University
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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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Catalysts (AREA)

Abstract

A kind of Fe (Co) SnO2The preparation method of combination electrode, is related to electrocatalytic oxidation methylene blue waste water technology field.By ferric acetyl acetonade（Or acetylacetone cobalt）, stannic chloride pentahydrate, high molecular polymer, organic solvent mix spinning solution is made；Fe (Co) Sn/PVP composite fiber precursors are made by electrostatic spinning；Precursor is carried out to heat treatment under air and prepares Fe (Co) SnO2Fiber；By the Fe prepared (Co) SnO2Catalysis electrode is made by the method for tabletting in fiber.Fe (Co) SnO wherein prepared using electrical spinning method2Fiber, due to the coupling of two-component transition metal, can obtain higher electro catalytic activity, with higher MB removal efficiencies, COD clearances and TOC clearances.

Description

A kind of Fe (Co)-SnO2The preparation method of combination electrode
Technical field
The present invention is the preparation field for belonging to Modified catalytic electrode, and in particular to Fe (Co)-SnO2The preparation of combination electrode Technology, and by its application in electrocatalytic oxidation methylene blue waste water.
Technical background
With the fast-developing of social economy while also with a series of environmental problem, especially for water resource Pollution directly threatens the existence of the mankind.Therefore, the processing for organic wastewater is gradually valued by people.At present, it is domestic The outer treatment technology for organic wastewater mainly includes Physical, bioanalysis and chemical method.Wherein chemical method is mainly wet method oxygen Change method, wet method catalytic oxidation, electrocatalytic oxidation etc..
Electrocatalytic oxidation is the method for the processing organic wastewater with difficult degradation thereby that recent decades gradually grow up.It can be in normal temperature Progress, mild condition under normal pressure, equipment is simple, floor space is small, operation and maintenance expense is relatively low, need not separately attach oxygenation Reducing agent, it is to avoid secondary pollution.The preparation of electrode is a step of most critical according to elctro-catalyst during electrocatalytic oxidation The location of in electrocatalysis device, two types can be divided into：One kind is that elctro-catalyst is located in solution；Another is electricity Catalyst is coupling on matrix, so that the catalyst electrode being made is used for electro-catalysis process.The preparation method of catalysis electrode is main It is electrodeposition process, sol-gal process, infusion process, thermal decomposition method etc..Anode material pattern prepared by this several method is difficult to control, And catalytic effect is less desirable, its electrode surface occurs passivation phenomenon and crack performance occurs to reduce catalysis drop The effect of solution.
Its pattern of the electrode catalyst prepared by method of electrostatic spinning continuously can be very good to solve this problem.Patent document It is used for Electrocatalysis Degradation organic waste 201610079959.8 disclosing and utilizing electrostatic spinning technique to prepare single metal oxides electrode Water.Transition metal（Such as Fe, Co）Deng being contacted in its atomic structure containing vacant d electronics with the electronics of reactant molecule, reach The purpose of molecule activation, so as to reduce the activation energy of reaction.Therefore, there is preferable electricity to urge for transition metal and its compound Change activity, and it is with low cost so the optimal selection as modified single metal oxides electrode, HeFei University of Technology Hu Caiju profits Co is prepared with electrodeposition process3O4/β-PbO2/ Ti electrode electro-catalysis degradation bisphenol-A waste water, from its SEM figures it can be seen that its electrode Surface occurs in that different degrees of cracking makes its coating shedding to reduce catalytic effect.
The content of the invention
For the defect of above prior art, the present invention seeks to propose in a kind of methylene blue waste water to oxidation COD and TOC clearances high Fe (Co)-SnO2The preparation method of combination electrode.
The present invention comprises the following steps：
1）First by polyvinylpyrrolidone（PVP）It is dissolved in organic solvent, then dissolves in the soluble metallic salt containing Fe or Co, obtains Spinning solution containing Fe or Co；
2）The spinning solution is subjected to electrostatic spinning, precursor is obtained；
3）Precursor is calcined, Fe (Co)-SnO is obtained2Composite nano fiber；
4）By Fe (Co)-SnO2Tabletting after composite nano fiber and auxiliary material mixing, obtains Fe (Co)-SnO2Combination electrode.
This method is mainly characterized by：Using electrostatic spinning technique, by dissolving in metal salt in presoma, then pass through again It is a series of to post-process the electrode for obtaining bimetallic oxide, for Electrocatalysis Degradation methylene blue waste water.
The present invention compared with prior art, with advantage once：
1st, the present invention is main prepares Fe (Co)-SnO using electrostatic spinning technique2As electrode, electrocatalytic oxidation methylene blue gives up Water.Wherein, Fe (Co)-SnO2Two-component nanofiber relative to one-component Fe bases or Sn base fibrous materials, due to the two Coupling, can obtain higher electro catalytic activity（Higher MB removal efficiencies, COD clearances and TOC can be obtained to remove Rate）.
2nd, relative to traditional electro-catalysis process, it is not necessary to separately attach reductant-oxidant, it is to avoid secondary pollution.
3rd, electrocatalytic oxidation organic wastewater is to carry out at normal temperatures and pressures, and operating condition is gentle, and electrolytic cell equipment is simple, always It must invest and relatively low with maintenance cost.
Further, the mixing quality of soluble metallic salt and polyvinylpyrrolidone of the present invention containing Fe or Co it Than for 1.25~2: 1.Mass ratio such as polyvinylpyrrolidone is excessive, then metal salt can not be dispersed in PVP well, Serious agglomeration occurs；Quality such as polyvinylpyrrolidone is very few, then the yield of metal oxide is too low.
The soluble metallic salt containing Fe is ferric acetyl acetonade（C15H21FeO6）And stannic chloride pentahydrate（SnCl4· 5H2O）Mixture, the ferric acetyl acetonade（C15H21FeO6）And stannic chloride pentahydrate（SnCl4·5H2O）Mixing quality ratio For 0.25~1: 1.
The soluble metallic salt containing Co is acetylacetone cobalt（C10H14CoO4）And stannic chloride pentahydrate（SnCl4· 5H2O）Mixture, the acetylacetone cobalt（C15H21FeO6）And stannic chloride pentahydrate（SnCl4·5H2O）Mixing quality ratio For 0.25~1: 1.
Mainly being easy to spinning using above metal salt, its metal oxide prepared has higher catalytic effect simultaneously. Tests prove that：Combination electrode using the two-component of both the above scheme is golden apparently higher than one-component to MB catalytic oxidation activities Belong to electrode.
The organic solvent is the mixed solvent of ethanol and N-N dimethylformamides, ethanol and N-N dimethylformamides Mixing quality ratio is 1: 1.Because ethanol has volatile, dissolubility is good and the advantages of low cost；And stannic chloride pentahydrate （SnCl4·5H2O）It is soluble in ethanol and is insoluble in N-N dimethylformamides（DMF）, ferric acetyl acetonade and acetylacetone cobalt are readily soluble In N-N dimethylformamides（DMF）It is insoluble in ethanol；All it is unfavorable for the molten of its metal salt when a certain component of mixed solvent is too high Solution.Further proved by experiment：Its two-component metal when the mixing quality ratio of ethanol and N-N dimethylformamides is 1: 1 Salt is most soluble.
The mixing quality ratio of the polyvinylpyrrolidone and organic solvent is 1: 9.The spinning solution viscosity of the proportions It is moderate, it is easy to spinning.
The temperature conditionss of the precursor calcining are 500 DEG C, and calcination time is 3h, and heating rate is 3 DEG C/min, under the conditions of being somebody's turn to do PVP can completely burn and can obtain the metal oxide of target valence state.
By Fe (Co)-SnO2After nanofiber and acetylene black, polytetrafluoroethylene (PTFE), ethanol mixing, sonicated 40min, In 70 DEG C of drying to pasty state, it is then coated with electrode matrix, tabletting after vacuum drying, the electrode prepared under the conditions of being somebody's turn to do has good Good stability.
The present invention prepares continuous Fe (Co)-SnO using electrostatic spinning technique2Composite nano fiber, then passes through pressure Piece couples with base electrode and prepares catalysis electrode, as anode, for electro-catalysis methylene blue waste water.
Brief description of the drawings
Fig. 1 is obtained Fe-SnO in example 12The SEM photograph of fiber.
Fig. 2 is obtained Co-SnO in example 62The SEM photograph of fiber.
Embodiment
First, example 1：
1st, spinning solution is prepared：
Weigh 2g polyvinylpyrrolidone（PVP）Add by 9g ethanol and 9g N-N dimethylformamides（DMF）Mixing group Into solvent in, stirring 12h then weighs 2g SnCl until solution is in clear shape4·5H2O is added in above-mentioned solution, is stirred Mix to solution clarification, weighing 0.5g ferric acetyl acetonade, stirring to solution clear, that is, obtain spinning solution.
2nd, precursor is prepared：
Spinning solution is fitted into 10mL syringe and carries out spinning control spinning condition, spinning voltage is 24kV, and temperature is 35 DEG C, Humidity is 30%, and it is 15cm to receive distance, and spinning speed is 0.2mm/min, and it is 25% to obtain ferric acetyl acetonade/stannic chloride pentahydrate Composite nano fiber.
3rd, Fe (Co)-SnO is prepared2Composite nano fiber：
Nanofiber is calcined into 3h with 3 DEG C/min programming rate in atmosphere at 500 DEG C, that is, obtains Fe-SnO2It is compound to receive Rice fiber.
Its SEM photograph is as shown in figure 1, as seen from Figure 1：The Fe-SnO of preparation2Composite fibre, diameter is thinner, average out to 200 nm, and diameter is evenly distributed.
4th, electrode material is prepared：
By the Fe-SnO of preparation2Nanofiber and acetylene black, polytetrafluoroethylene (PTFE), ethanol are using mass ratio as 80:10:5 ratio is mixed 24h, sonicated 40min are stirred after conjunction.It is well mixed, dries to pasty state, is then coated with electrode base at 70 DEG C On body, 24h is dried in vacuo, then with tablet press machine in 10MPa pressure lower sheetings, Fe-SnO is made2Nanofiber passes through tabletting system Into electrode material.
5th, apply：
By obtained Fe-SnO2Electrode is used for electro-catalysis methylene blue waste water：With fibrous Fe-SnO2Electrode as anode, Copper coin is negative electrode, 0.25mol/L NaNO3For electrolyte, interelectrode distance is 2cm, and current density is 20mA/cm2, electricity urges The environment temperature of change is 30 DEG C, and the initial pH of solution is 7, the concentration of organic wastewater be the 200mg/L electro-catalysis times be 5h.Wherein The clearance that the clearance that the percent of decolourization of electro-catalysis methylene blue waste water is 80.3%, COD is 40.3%, TOC is 52.1%.
2nd, example 2：
It is similar with the step in example 1, the 0.5g weighed ferric acetyl acetonade is only increased into 1g, Fe-SnO is made2Nanowire Dimension.
Final Fe-SnO2The removal efficiency that the electro-catalysis methylene blue waste water of electrode material is made up of tabletting for nanofiber is The clearance that 84.8%, COD clearance are 46.5%, TOC is 58.3%.
3rd, example 3：
It is similar with the step in example 1, the 0.5g weighed ferric acetyl acetonade is only increased into 1.5g, be made ferric acetyl acetonade with The mass ratio of stannic chloride pentahydrate is 75% Fe-SnO2Nanofiber, the removal efficiency of electro-catalysis methylene blue waste water is 93.9%, The clearance that COD clearance is 63.3%, TOC is 74.3%.
4th, example 4：
It is similar with the step in example 1, the 0.5g weighed ferric acetyl acetonade is only increased into 2g, Fe-SnO is made2Nanowire Dimension.
Final Fe-SnO2The removal efficiency that the electro-catalysis methylene blue waste water of electrode material is made up of tabletting for nanofiber is The clearance that 82.9%, COD clearance are 44.2%, TOC is 54.3%.
5th, example 5：
It is similar with the step in example 1, only change the 0.5g weighed ferric acetyl acetonade into 0.5g acetylacetone cobalts, Co- is made SnO2Nanofiber.
Final Co-SnO2The removal efficiency that the electro-catalysis methylene blue waste water of electrode material is made up of tabletting for nanofiber is The clearance that 91.3%, COD clearance are 58.2%, TOC is 70.2%.
6th, example 6：
It is similar with the step in example 1, only change the 0.5g weighed ferric acetyl acetonade into 1g acetylacetone cobalts, Co- is made SnO2Nanofiber.
Co-SnO is obtained after calcining2The SEM photograph of composite nano fiber is visible：Diameter is thicker, averagely reaches 500nm, And diameter is evenly distributed.
Final Co-SnO2The removal efficiency that the electro-catalysis methylene blue waste water of electrode material is made up of tabletting for nanofiber is The clearance that 94.5%, COD clearance are 66.4%, TOC is 77.4%.
7th, example 7：
It is similar with the step in example 1, only change the 0.5g weighed ferric acetyl acetonade into 1.5g acetylacetone cobalts, Co- is made SnO2Nanofiber.
Final Co-SnO2The removal efficiency that the electro-catalysis methylene blue waste water of electrode material is made up of tabletting for nanofiber is The clearance that 86.3%, COD clearance are 52.2%, TOC is 61.3%.
8th, example 8：
It is similar with the step in example 1, only change the 0.5g weighed ferric acetyl acetonade into 2g acetylacetone cobalts, Co- is made SnO2Nanofiber.
Final Co-SnO2The removal efficiency that the electro-catalysis methylene blue waste water of electrode material is made up of tabletting for nanofiber is The clearance that 83.3%, COD removal efficiency are 49.3%, TOC is 58.6%.

Claims (8)

1. a kind of Fe (Co)-SnO2The preparation method of combination electrode, comprises the following steps：
1）Prepare the spinning solution containing Fe or Co；
2）The spinning solution is subjected to electrostatic spinning, precursor is obtained；
3）Precursor is calcined, Fe (Co)-SnO is obtained2Composite nano fiber；
4）By Fe (Co)-SnO2Tabletting after composite nano fiber and auxiliary material mixing, obtains Fe (Co)-SnO2Combination electrode；
It is characterized in that：In the step 1）In, first polyvinylpyrrolidone is dissolved in organic solvent, then dissolves in containing Fe or Co Soluble metallic salt, obtain the spinning solution containing Fe or Co.
2. preparation method according to claim 1, it is characterised in that：The soluble metallic salt containing Fe or Co and poly- second The ratio between mixing quality of alkene pyrrolidone is 1.25~2: 1.
3. preparation method according to claim 2, it is characterised in that：The soluble metallic salt containing Fe is acetylacetone,2,4-pentanedione The mixture of iron and stannic chloride pentahydrate, the mixing quality ratio of the ferric acetyl acetonade and stannic chloride pentahydrate is 0.25~1: 1.
4. preparation method according to claim 2, it is characterised in that：The soluble metallic salt containing Co is acetylacetone,2,4-pentanedione The mixture of cobalt and stannic chloride pentahydrate, the mixing quality ratio of the acetylacetone cobalt and stannic chloride pentahydrate is 0.25~1: 1.
5. preparation method according to claim 1, it is characterised in that：The organic solvent is ethanol and N-N dimethyl methyls The mixing quality ratio of the mixed solvent of acid amides, ethanol and N-N dimethylformamides is 1: 1.
6. preparation method according to claim 5, it is characterised in that：The polyvinylpyrrolidone and organic solvent it is mixed It is 1: 9 to close mass ratio.
7. preparation method according to claim 1, it is characterised in that：The calcining heat of precursor is 500 DEG C, and calcination time is 3h, heating rate is 3 DEG C/min.
8. preparation method according to claim 1, it is characterised in that：The step 4）In, by Fe (Co)-SnO2Composite Nano After fiber and acetylene black, polytetrafluoroethylene (PTFE), ethanol mixing, after sonicated 40min, 70 DEG C of drying are then coated with to pasty state In on electrode matrix, tabletting after vacuum drying.
CN201710376231.6A 2017-05-25 2017-05-25 A kind of Fe (Co) SnO2The preparation method of combination electrode Pending CN107055701A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850641A (en) * 2006-05-26 2006-10-25 上海大学 Method for preparing carbon nano tube/tin dioxide composite electro catalytic electrode
CN104319372A (en) * 2014-11-14 2015-01-28 湖南大学 Convenient method for preparing binder-free stannic oxide/carbon fibrofelt for negative pole of high-performance lithium ion battery
CN105478102A (en) * 2016-02-05 2016-04-13 扬州大学 Method for preparing catalyst for electrical catalytic degradation of organic wastewater

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850641A (en) * 2006-05-26 2006-10-25 上海大学 Method for preparing carbon nano tube/tin dioxide composite electro catalytic electrode
CN104319372A (en) * 2014-11-14 2015-01-28 湖南大学 Convenient method for preparing binder-free stannic oxide/carbon fibrofelt for negative pole of high-performance lithium ion battery
CN105478102A (en) * 2016-02-05 2016-04-13 扬州大学 Method for preparing catalyst for electrical catalytic degradation of organic wastewater

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
逯瑶等: "第一性原理研究Fe掺杂SnO2材料的光电性质", 《物理学报》 *

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