CN1900365A - Method for preparing ferrate by electric generating method and its special electrolytic bath - Google Patents
Method for preparing ferrate by electric generating method and its special electrolytic bath Download PDFInfo
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- CN1900365A CN1900365A CN 200610101011 CN200610101011A CN1900365A CN 1900365 A CN1900365 A CN 1900365A CN 200610101011 CN200610101011 CN 200610101011 CN 200610101011 A CN200610101011 A CN 200610101011A CN 1900365 A CN1900365 A CN 1900365A
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Abstract
The present invention relates to an electricity generation method to prepare ferrate method and special electrolytic bath. Said Electrolytic bath adopts double diaphragm twin cathode cylinder trough solid structure composed of cathode bar, internal partition film tube, anode tube, outside cylindrical diaphragm, outside cathode tube and trough solid outer cylinder, to form one anode corresponding inside and outside two cathodes, double diaphragm dividing electrolytic bath into two cathode chambers and two anode chambers..Said invention utilizes double diaphragm twin cathode cylinder trough solid electrolytic bath to prepare ferrate, adding NaOH or KOH electrolyte, controlling electrolytic bath liquid temperature range at 25-30 degree centigrade, current density 30 ma/cm 2, adding 0.1-0.25 per cent NaCl or KCl, electrolyzing for 4-6 hr to obtain 0.07 mol/L FeO 42-.Said structure can make anode inside and outside two surfaces being fully utilized, raising current efficiency and resultant concentration, suitable for preparing electrogenesis novel water treatment agent ferrate.
Description
Technical field
The present invention relates to a kind of electric method of formation and prepare the method for ferrate and special-purpose in the preparation electrolyzer thereof, belong to electrochemical field in the chemical industry.
Technical background
In the iron cpd that has made at present, Tie Tong often exists with the form of Fe (II) and Fe (III), but it can be oxidized to sexavalence iron under the effect of strong oxidizer.Ferrate is iron+6 valency compounds, is the oxysalt of the iron that exists with high valence state form, and its chemical formula is MxFeO
4)(M: basic metal or alkaline-earth metal).
Ferrate is a kind of strong oxidizer, in acidic solution as the sexavalence compound of iron, its redox potential is up to 2.2V, and in basic solution, its redox potential is 0.72V, the effective organism in the many trade effluents of oxidative degradation, the Fe that the reduction back generates
3+Hydrolysate Fe (OH)
3Be a kind of flocculation agent, and have good adsorption effect.Therefore, ferrate has the multiple function of oxidation, absorption and flocculation, is a kind of ideal water treatment agent, has important development and application values.
Because the special chemical property of ferrate, it has very high using value in water treatment procedure, be a kind ofly to integrate usefulness such as oxidation, flocculation, virus killing, and the high-efficiency multi-function water treatment compound that has no side effect.In addition, ferrate also can be used as the oxygenant in some organic synthesis, and there is not secondary pollution in its reduzate to environment; As the positive electrode active materials of green power supply, have higher electrode potential and specific capacitance etc. again.Because ferrate in the tempting application prospect in these fields, makes the method for its preparation and processing condition become the important subject of high-technology field in recent years.
The preparation technology of ferrate can be divided into dry method, wet method, electrolytic process three classes.Dry method claims the high-temperature fusion oxidation style again, is the method for using the earliest for preparing ferrate.This method adopts under the highly basic existence condition, and oxygenants such as saltpetre or superoxide can be oxidized to ferrate with the oxide compound of molysite or iron under hot conditions.High-temperature oxidation is difficult to realization in common laboratory, and has potential safety hazard, so development prospect is little; Wet method claims the hypochlorite oxidation style again.Preparation ferrate principle is to feed Cl in the NaOH solution
2Gas also makes it fully saturated, generates NaClO, then under strong alkaline condition, and the NaClO Oxidation of Fe
3+[as Fe (NO
3)
3, FeCl
3] one-tenth Na
2FeO
4As the synthetic K of desire
2FeO
4, because K
2FeO
4Solubleness in the NaOH strong solution compares Na
2FeO
4Solubleness in the NaOH strong solution is little, therefore can make Na
2FeO
4Make by replacement(metathesis)reaction with KOH.The hypochlorite oxidation style can obtain solid-state purified ferrate, but the consumption of raw material thing is too many, and preparation process is long, therefore need and shorten on the preparation flow haveing breakthrough at the raising raw material availability; The principle that electrolytic process prepares ferrate is, under the condition of energising, and in strongly basic medium, the oxidized generation of anode iron FeO
4 2-, negative electrode generation evolving hydrogen reaction, anode takes place with analysing the oxygen side reaction simultaneously.Electrolytic process preparation condition gentleness, ingredient requirement is low, and the ferrate solution of electrolytic preparation can now-making-now-using (as water conditioner), but it is low that the subject matter of electrolytic process is production concentration, current efficiency is low and unstable, maximum current efficient is difficult to stable the maintenance, is subject to the influence of factors such as electromotive force, current density, temperature.Therefore will obtain high as far as possible ferrate concentration and then need keep high as far as possible current efficiency in long-time electrolytic, the selection of anode material, reasonably cell construction etc. is the emphasis of developing.
Electrolytic process prepares in the ferrate based on metallic iron anode electrolysis method, and used electrolyzer once had two types of no diaphram tank, physical membrane grooves in the technology.The control mode of electrolytic solution also has single-channel type and flowing-type.
At present, the electrolytic process electrolyzer for preparing in the ferrate technology to be adopted has or not diaphram tank, physical membrane groove, ion diaphragm groove etc.Because ferrate is a strong oxidizer, in electrolytic process,, make it form layer oxide film and cover anode surface, thereby stoped the dissolving of iron the iron of oxidation anode surface, reduced the current efficiency of electrolysis preparation of ferrate.Adopt dull and stereotyped iron anode,, generally can only obtain rarer ferrate solution and lower current efficiency because the electrode surface utilization ratio is low and the surface current problem of uneven distribution.Therefore, anode material choose with the improvement of cell construction significant concerning the electrolytic preparation ferrate.
Compare with high-temperature fusion oxidation style, hypochlorite oxidation style, electrolytic process is because its raw material consumption is few, easy to operate, the ferrate that obtains can directly be used for water treatment continuously, avoided the problem of the storage aspect that the unstable of loaded down with trivial details purifying technique and high ferro itself brings, wide application prospect has been arranged.
Strong oxidizer as a kind of green, safety, ferrate is showing great application prospect as fields such as chemical power source positive active material, selective oxidation agent and water conditioners, but owing to lack the special electrolytic tank that is used to prepare ferrate, make electrolytic process prepare the ferrate method and do not obtain industrial applications always at present.
The basic structural unit of having formed electrolyzer by negative electrode, anode, barrier film, insulated enclosure pad and utmost point frame etc.Along with development of technology and development, traditional electrolyzer develops out the MA cell diaphragm cell with metal anodes of monopolar ion membrane electrolyzer, multipole type pump circulation ion-exchange membrane electrolyzer, bipolar type natural-circulation ion-exchange membrane electrolyzer, multipole type natural circulation high current density ion-exchange membrane electrolyzer, a bipolar type ion-exchange membrane electrolyzer and all size of all size, do not let alone how to develop but have, its ultimate principle and basic structure do not change, and its profile is still based on square pond shape groove.Aspect electrode, it is anode or negative electrode that nothing is appointed, based on traditional bar-shaped, sheet, tabular; The quantitative aspects of electrode is even number usually, and anode and cathode is corresponding one by one; Aspect tank room, do not have to appoint and whether to have adopted barrier film, or two Room, three cell structures, all belong to traditional tandem arranged side by side.Above-mentioned all structures, though have different advantages separately, but the skewness of inside and outside two surface charges of electrode, the one side utilization ratio high and opposing with respect to the electrode material surface utilization ratio of different in nature electrode is low, simultaneously, electromotive force potential variation non-rectilinear gradient type in the electrolytic solution, the density of electric current also is difficult to homogeneous, thus the generation concentration and the product yield of current efficiency and preparation product when influencing electrolysis.
Formation and electrolysis that the present invention investigates different iron-based material oxide films generate the difference of ferrate current efficiency, and with two barrier film double cathode round tube type electrolysis ferrates, have obtained the ferrate solution of high density, have improved electrolytic current efficiency.
1, dull and stereotyped cast iron anodic electrolyzer
Dull and stereotyped cast iron anodic electric tank cathode is the plate graphite electrode, and anode is the dull and stereotyped ferroelectric utmost point, and apparent area is 15cm
2Separate with cationic exchange membrane between anolyte compartment and the cathode compartment, the electrolytic solution in anode and the cathode compartment is all the NaOH solution of 14mol/L.Anolyte compartment's volume is 200ml, and the cathode compartment volume is 150ml.Must stir by antianode liquid during electrolysis.
2, cylinder double cathode electrolytic tank
For overcoming the low and surface current problem of uneven distribution of plate electrode surface utilization ratio, the present invention adopts the concentric drums cell construction, two barrier films, and inside and outside two negative electrodes of anode correspondence, the Ag/AgCl electrode is measured anode potential as reference electrode.With DF1720SB5A type D.C. regulated power supply as electrolysis power.Adopt the electrolyzer of this kind structure that inside and outside two surfaces of anode evenly and are fully utilized, thereby reach the purpose that improves current efficiency and ferrate generation concentration.
Summary of the invention
Purpose of the present invention: (one) is to overcome the deficiency in the existing design, provide electrolytic solution distribution of current between a kind of anode and cathode evenly, help that inside and outside two surfaces of anode effectively play a role and the two barrier film double cathode electrolytic tanks of a kind of novel cylinder of being fully used, thereby reach the purpose that improves current efficiency; (2) utilize this specific two barrier film double cathode round tube type electrolyzers, prepare product and generate concentration and the product yield ferrate higher than plain electrolysers.
The objective of the invention is to realize through following scheme.
(1) design of special electrolytic tank
The present invention adopts the cell construction of two barrier film double cathodes, round tube type cell body.The cell body outward appearance is cylindric, inner bottom surface is provided with 5 equidistant concentric circular grooves, the circular groove of circle centre position is used for fixing the inner cathode rod, what outwards be provided with at interval successively is inner septum tube, anode tube, outer cylindrical diaphragm, outer cathode tube and cell body urceolus, forms the round tube type cell construction that an anode correspondence inside and outside two negative electrodes, two barrier films are divided into electrolyzer 2 cathode compartments and 2 anolyte compartments.The cell body of electrolyzer adopts the PVC material to make, the inner cathode rod adopts graphite material to make, the outer cathode tube adopts the stainless steel sheet material that has uniform micro, inside and outside two barrier films adopt the Nafion117 cationic exchange membrane, anode is selected grey cast iron (trade mark HT200) for use, simultaneously be distributed with uniform aperture at anode surface, thereby but make inside and outside electrolytic solution unrestricted flow, but both sides resultant uniform distribution.
(2) prepare the method for ferrate
When the electrolyzer of the two barrier film double cathodes of utilization, round tube type cell body prepares ferrate, add NaOH or the KOH electrolytic solution of 14mol/L, 25～30 ℃ of temperature ranges of control cell liquid are connected with the mains, and its current density is 30mA/cm
2, adding 0.1～0.25%NaCl or KCl, electrolysis 4～6h gets the FeO of 0.07mol/L
4 2-
The electrolyzer that adopts this structure design to go out, inside and outside two surfaces of anode evenly and are fully utilized, thereby reach the concentration that improves current efficiency and resultant, be applicable to various electrochemical production inorganic salt, the organic salts of passing through, be particularly useful for making electricity and generate novel water conditioner ferrate.
Description of drawings
Fig. 1 is a cell construction synoptic diagram of the present invention.
Fig. 2 is that cylindrical diaphragm of the present invention launches the back plane structural representation.
Among Fig. 1,1 is the graphite cathode rod, is positioned at the central position of electrolyzer; The 2nd, the inner septum tube is made up of macrolattice intermediate plate and barrier film that the PVC material is made; The 3rd, the anode tube adopts grey cast iron (trade mark HT200) to make, and its surface arrangement has uniform aperture; The 4th, outer cylindrical diaphragm, its material is identical with the inner septum tube with structure; The 5th, the outer cathode tube, the 6th, the cell body outer side wall of electrolyzer, adopt the PVC material to make, the inner bottom surface of cell body is provided with equidistant concentric circular grooves, cathode bar 1, inner septum tube 2, anode tube 3, outer cylindrical diaphragm 4, outer cathode tube 5 embed wherein successively, and electrolyzer is divided into 2 cathode compartments and 2 anolyte compartments naturally.
Among Fig. 2, the 7th, by the macrolattice intermediate plate that the PVC material is made, a cylindrical diaphragm is made up of two intermediate plates, and the 8th, ion-exchange membrane is fixed between two intermediate plates, and the ion-exchange membrane that the utility model adopts is the Nafion117 cationic exchange membrane.
Embodiment
The invention will be further described with by way of example below in conjunction with accompanying drawing.
(1) design of special electrolytic tank
Adopt the PVC material, utilize the method for injection moulding, produce the cell body of electrolyzer, its outward appearance is cylindric, inner bottom surface is provided with 5 equidistant concentric circular grooves, the circular groove of circle centre position is used for fixing inner cathode rod 1, and inner septum tube 2, anode tube 3, outer cylindrical diaphragm 4, outer cathode tube 5 can embed in the groove successively, and electrolyzer is divided into 2 cathode compartments and 2 anolyte compartments naturally.Inner cathode rod 1 adopts graphite material to make, and the outer cathode rod adopts stainless (steel) wire.Anode is selected round shape grey cast iron (trade mark HT200) for use, and is loose porous owing to having on the grey cast iron structure, and bigger specific surface area effectively is provided, and wherein contained Fe
3C helps the electrolysis of iron, is distributed with the uniform small pores that diameter is 4mm at anode surface simultaneously, thereby but make inside and outside electrolytic solution unrestricted flow, but the ferrate uniform distribution that inside and outside both sides generate.The high 5cm of cast iron anode, external diameter 5.5cm, barrel is thick to be 3mm, the anode apparent area is 37.1cm
2, anolyte compartment's volume is 250mL.Outer cathode chamber volume is 280mL, and inner cathode chamber volume is 20mL.Electrolytic solution in anode and the cathode compartment is all 14mol/LNaOH solution.
A cylindrical diaphragm is made up of two intermediate plates and an exchange membrane, is provided with corresponding primary and secondary shape clasp between intermediate plate and the intermediate plate, sandwich exchange membrane between two intermediate plates after, firmly with two intermediate plate fastenings, the macrolattice intermediate plate can be rolled into cylindric.The 8th, ion-exchange membrane is fixed between two intermediate plates, and the ion-exchange membrane that the utility model adopts is the Nafion117 cationic exchange membrane.Adopt the Nafion117 cationic exchange membrane when being used to prepare ferrate, can prevent the FeO that generates
4 2-Enter negative electrode and be reduced consumption.The Ag/AgCl electrode is measured anode potential as reference electrode.With DF1720SB5A type D.C. regulated power supply as electrolysis power.
(2) prepare the method for ferrate
During the preparation ferrate, add the NaOH 500ml electrolytic solution of 14mol/L, 25 ℃ of temperature of control cell liquid connect 30mA/cm
2Current density, add 0.25%NaCl 30ml, electrolysis 4h gets the Na of 0.07mol/L
2FeO
4
(1) design of special electrolytic tank
Cell construction is as described in the embodiment 1.
(2) prepare the method for ferrate
During the preparation ferrate, add the KOH 515ml electrolytic solution of 14mol/L, 30 ℃ of temperature of control cell liquid connect 30mA/cm
2Current density, add 0.25%NaCl 35ml, electrolysis 6h gets the K of 0.07mol/L
2FeO
4
(1) design of special electrolytic tank
Cell construction is as described in the embodiment 1.
(2) prepare the method for ferrate
During the preparation ferrate, add the NaOH 480ml electrolytic solution of 14mol/L, 28 ℃ of temperature of control cell liquid connect 30mA/cm
2Current density, add 0.25%KCl 25ml, electrolysis 5h gets the Na of 0.07mol/L
2FeO
4
(1) design of special electrolytic tank
Cell construction is as described in the embodiment 1.
(2) prepare the method for ferrate
During the preparation ferrate, add the KOH 500ml electrolytic solution of 14mol/L, 30 ℃ of temperature of control cell liquid connect 30mA/cm
2Current density, add 0.25%KCl 30ml, electrolysis 5h gets the K of 0.07mol/L
2FeO
4
Claims (6)
1, a kind of electrolyzer that is used for the special use of electric method of formation electrolytic preparation ferrate, it is characterized in that being provided with in the electrolyzer two cylindrical diaphragms and double cathode, form the two barrier film double cathode electrolytic tanks of round tube type that inside and outside two negative electrodes of an anode correspondence, two cylindrical diaphragm are divided into electrolyzer 2 cathode compartments and 2 anode cell configuration.
2, electrolyzer according to claim 1 is characterized in that the cell body outward appearance is round tube type, and inner bottom surface is provided with 5 equidistant concentric circular grooves.
3, electrolyzer according to claim 2 is characterized in that the groove center on the electrolyzer inner bottom surface groove is a cathode bar, and what outwards embed at interval successively is inner septum tube, anode tube, outer cylindrical diaphragm, outer cathode tube and cell body urceolus.
4, electrolyzer according to claim 1, the cell body that it is characterized in that electrolyzer formation electrolyzer adopts the PVC material to make, the inner cathode rod adopts graphite material to make, the outer cathode tube adopts the stainless steel sheet material that has uniform micro, inside and outside two barrier films adopt the Nafion117 cationic exchange membrane, and anode is selected grey cast iron for use.
5, electrolyzer according to claim 1 is characterized in that the anode surface of electrolyzer is distributed with uniform aperture.
6, a kind ofly utilize two barrier film double cathode round tube type electrolyzers electricity method of formation to prepare the method for ferrate, it is characterized in that adding the NaOH of 14mol/L or KOH as electrolytic solution in electrolyzer, the control flume temperature passes to 30mA/cm in 25～30 ℃ of temperature ranges
2Current density, add 0.1～0.25%NaCl or KCl, electrolysis 4～6h gets the FeO4 of 0.07mol/L
2-
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101187028B (en) * | 2007-06-27 | 2010-04-14 | 上海电力学院 | Potassium ferrate preparation method |
| CN101713078A (en) * | 2009-09-22 | 2010-05-26 | 上海市政工程设计研究总院 | Device and method for preparing potassium ferrate through electrolysis |
| CN102286747A (en) * | 2011-09-02 | 2011-12-21 | 广州市天承化工有限公司 | Recycling and regeneration of microetching liquid and recycling system of metal copper |
| CN102925919A (en) * | 2012-11-23 | 2013-02-13 | 哈尔滨工业大学 | On-line addition device for three-dimensional electrode electrochemical oxidation ferrate solution |
| CN103938220A (en) * | 2014-04-29 | 2014-07-23 | 北京化工大学 | Method for preparing hydrazobenzene compound through adopting electrolysis method, and electrolytic device |
| CN105040023A (en) * | 2015-06-29 | 2015-11-11 | 浙江大学 | Preparation method of liquid potassium ferrate by utilizing ultrasonic electrolysis |
| CN105386117A (en) * | 2015-11-24 | 2016-03-09 | 常州乐奥医疗科技有限公司 | Electrochemical polishing device and method for support |
| CN106048649A (en) * | 2016-08-05 | 2016-10-26 | 华侨大学 | Combined electrolytic tank for ferrate preparation |
| CN107022767A (en) * | 2017-05-10 | 2017-08-08 | 东北大学 | A kind of device that hydroxide is prepared for electrolytic metal chloride |
| CN110129819A (en) * | 2019-06-05 | 2019-08-16 | 浙江工业大学 | A kind of new-type electrolytic preparation optimization method of potassium ferrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101187028B (en) * | 2007-06-27 | 2010-04-14 | 上海电力学院 | Potassium ferrate preparation method |
| CN101713078A (en) * | 2009-09-22 | 2010-05-26 | 上海市政工程设计研究总院 | Device and method for preparing potassium ferrate through electrolysis |
| CN102286747A (en) * | 2011-09-02 | 2011-12-21 | 广州市天承化工有限公司 | Recycling and regeneration of microetching liquid and recycling system of metal copper |
| CN102925919A (en) * | 2012-11-23 | 2013-02-13 | 哈尔滨工业大学 | On-line addition device for three-dimensional electrode electrochemical oxidation ferrate solution |
| CN103938220B (en) * | 2014-04-29 | 2016-08-24 | 北京化工大学 | Electrolysis prepares method and the electrolysis unit of hydrodiazo benzene-like compounds |
| CN103938220A (en) * | 2014-04-29 | 2014-07-23 | 北京化工大学 | Method for preparing hydrazobenzene compound through adopting electrolysis method, and electrolytic device |
| CN105040023A (en) * | 2015-06-29 | 2015-11-11 | 浙江大学 | Preparation method of liquid potassium ferrate by utilizing ultrasonic electrolysis |
| CN105386117A (en) * | 2015-11-24 | 2016-03-09 | 常州乐奥医疗科技有限公司 | Electrochemical polishing device and method for support |
| CN106048649A (en) * | 2016-08-05 | 2016-10-26 | 华侨大学 | Combined electrolytic tank for ferrate preparation |
| CN106048649B (en) * | 2016-08-05 | 2018-01-09 | 华侨大学 | A kind of combined electrolysis bath for being used to prepare ferrate |
| CN107022767A (en) * | 2017-05-10 | 2017-08-08 | 东北大学 | A kind of device that hydroxide is prepared for electrolytic metal chloride |
| CN107022767B (en) * | 2017-05-10 | 2019-04-23 | 东北大学 | A kind of device preparing hydroxide for electrolytic metal chloride |
| CN110129819A (en) * | 2019-06-05 | 2019-08-16 | 浙江工业大学 | A kind of new-type electrolytic preparation optimization method of potassium ferrate |
| CN110129819B (en) * | 2019-06-05 | 2020-08-04 | 浙江工业大学 | Electrolytic preparation optimization method of potassium ferrate |
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