CN112746287A - Method for preparing liquid sodium ferrate based on electrolytic method and electrolytic bath thereof - Google Patents
Method for preparing liquid sodium ferrate based on electrolytic method and electrolytic bath thereof Download PDFInfo
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Abstract
The invention provides a method for preparing liquid sodium ferrate based on an electrolytic method, which comprises the following steps: step 1, softening water by using a softener to remove calcium, magnesium and other ions to obtain softened water; step 2, adding the softened water into a stirrer with a sodium hydroxide solution and a potassium chloride solution, stirring at a set speed, and mixing uniformly to prepare an electrolyte; step 3, adding the electrolyte into a condenser for condensation, and controlling the temperature to be 30-40 ℃ to obtain the condensed electrolyte; and 4, adding the condensed electrolyte into an electrolytic cell, and electrolyzing the electrolyte for a certain time at a set current density to obtain a sodium ferrate solution. The present invention also provides an electrolytic cell comprising: the groove body is in a cuboid shape; the three partition plates are arranged in the tank body and partition the tank body into four areas; and four tank covers respectively placed at the top of the tank body and used for covering the four areas.
Description
Technical Field
The invention belongs to the field of electrochemistry, and particularly relates to a method for preparing liquid sodium ferrate based on an electrolytic method and an electrolytic cell thereof.
Background
With the high development of global industrialization, the problem of water pollution is becoming more serious, and the traditional water treatment agent has been proved to generate a series of byproducts harmful to organisms, so that the development of a new water treatment agent is urgently needed. Ferrate is the highest valence compound of iron, and under acidic condition, its standard oxidation-reduction potential is 2.20V, and is higher than all current disinfectants applied in water treatment, and is a strong oxidizing substance. In the oxidation process, ferrate is reduced into trivalent ferric salt with flocculation, and can efficiently remove tiny suspended matters in water. In addition, it is possible to oxidize away, for example, hydrogen sulfide (H)2S), methyl mercaptan (CH)3SH), methylthio (CH)3)2S), ammonia (NH)3) And the like, and converts the malodorous substances into safe and tasteless substances. In a word, the ferrate is a novel high-efficiency green water treatment agent with the functions of oxidation, adsorption, flocculation, coagulation aiding, sterilization, algae removal, turbidity removal, decoloration, deodorization and the like, and has great application prospect.
Theoretically, ferrate (FeO)4 2-) The anion can be substituted with many metal cations and some metalloid cations (e.g., NH)4 +，N(C4H9)4+) Simple salts of oxyacids are formed, but it is difficult to actually produce measured amounts of ferrate, and more difficult to produce ferrate in high purity or crystalline form. At present, ferrate prepared at home and abroad is mainly potassium ferrate and sodium ferrate, and three methods are mainly adopted: dry oxidationProcesses, wet oxidation processes and electrolysis processes.
Dry oxidation, also known as melt oxidation, is based on the principle of oxidizing peroxides (e.g., Na) in a high temperature caustic environment2O2Or K2O2) With elemental iron or iron-containing compounds (e.g. FeSO)4) High temperature solid (or melt) phase reactions occur to produce ferrate. The method needs conditions of high temperature, high pressure, oxygen deficiency and the like, needs external large-scale accessory equipment, is difficult to realize industrial production, and is rarely adopted at present.
The wet oxidation method is also called hypochlorite oxidation method, and the principle is that under the condition of strong alkali, hypochlorite (such as KClO and NaClO) oxidizes a trivalent iron source into ferrate ions to generate ferrate. The ferrate prepared by the method has low purity, and can be obtained only by a series of purification operations. In addition, this method has some disadvantages: such as complicated practical operation procedures, low-temperature conditions, use of organic solvents such as ether harmful to human bodies during purification, and the presence of chlorine for the preparation and decomposition of hypochlorite, have high requirements on the air tightness and corrosion resistance of the device, so that the method is only used for preparing ferrate in a laboratory and does not realize industrial application.
The electrolytic method for preparing ferrate is one of the hot spots in recent research, and the principle is that an iron anode is oxidized into ferrate ions in a strong alkaline electrolytic cell, and the reaction process is as follows:
and (3) anode reaction:
and (3) cathode reaction: 2H2O+2e-→H2↑+2OH-
The current efficiency determines the power consumption and the ferrate concentration, and the main factors influencing the current efficiency include the electrolyte composition, the concentration, the temperature, the current density on the surface of the anode and the like. In the electricityDuring the solution process, the iron electrode is gradually formed by Fe on the surface2O3/Fe3O4The bimolecular film is passivated, so that the current efficiency is reduced; in addition, hydrogen gas with reduction effect is generated in the electrolysis, and the purity of the generated ferrate is influenced if the hydrogen gas is not removed in time.
To sum up: compared with the former two methods, the electrolysis method has the characteristics of good equipment systematicness, less raw material consumption, flexibility, convenience, no secondary pollution and the like, is more suitable for the technical process of on-site preparation and addition, and is worthy of deep research.
Disclosure of Invention
The present invention is made to solve the above problems, and an object of the present invention is to provide a method for producing liquid sodium ferrate by an electrolytic method and an electrolytic cell thereof.
The invention provides a method for preparing liquid sodium ferrate based on an electrolytic method, which is characterized by comprising the following steps: step 1, softening water by using a softener to remove calcium, magnesium and other ions to obtain softened water; step 2, adding the softened water into a stirrer with a sodium hydroxide solution and a potassium chloride solution, stirring at a set speed, and mixing uniformly to prepare an electrolyte; step 3, adding the electrolyte into a condenser for condensation, and controlling the temperature to be 30-40 ℃ to obtain the condensed electrolyte; and 4, adding the condensed electrolyte into an electrolytic cell, and electrolyzing the electrolyte for a certain time at a set current density to obtain a sodium ferrate solution.
The method for preparing liquid sodium ferrate based on the electrolysis method provided by the invention can also have the following characteristics: wherein, in the step 2, the concentration of the potassium chloride solution is 1 mol.L-1The concentration of the sodium hydroxide hydrolysate is 16 mol.L-1The stirring speed is 120 to 180 rad.min-1。
The method for preparing liquid sodium ferrate based on the electrolysis method provided by the invention can also have the following characteristics: wherein, in the step 4, the current density is 50mA/cm2～200mA/cm2The electrolysis duration is 1.5 h-3 h.
The present invention also provides an electrolytic cell for use in the above-mentioned method for producing liquid sodium ferrate by electrolysis, for electrolyzing an electrolyte, which has the characteristics comprising: the groove body is in a cuboid shape; the three partition plates are arranged in the tank body and partition the tank body into four areas; and the four tank covers are respectively placed at the top of the tank body and used for covering the four areas, wherein the lower parts of the four areas are communicated, the first area is a liquid level height control area, the second area, the third area and the fourth area are electrolysis areas, each electrolysis area is provided with five pairs of grooves, each five pairs of grooves comprise three pairs of anode grooves and two pairs of cathode grooves, the number of the inserted electrode plates is determined according to needs, and no diaphragm is arranged between the electrode plates.
The method for preparing liquid sodium ferrate based on the electrolysis method provided by the invention can also have the following characteristics: wherein, the groove body, the groove cover and the clapboard are made of PP materials which are resistant to the corrosion of alkali liquor.
The method for preparing liquid sodium ferrate based on the electrolysis method provided by the invention can also have the following characteristics: wherein, install level sensor on the cell lid in first region for automated inspection liquid level height, all install a fan on the cell lid in second region, the cell lid in third region and the cell lid in fourth region for get rid of the hydrogen that has reducibility that produces in the electrolysis process.
The method for preparing liquid sodium ferrate based on the electrolysis method provided by the invention can also have the following characteristics: when electrolysis is carried out in the electrolytic tank, the current needs to be reversed every 0.5h for eliminating the passive film on the wire netting.
Action and Effect of the invention
The method for preparing liquid sodium ferrate based on the electrolytic method has the characteristics of simplicity, convenience, low raw material consumption, capability of degrading pollutants, good degradation effect, no secondary pollution and the like, and is more suitable for the technical processes of on-site preparation and addition.
In addition, the electrolytic cell has simple structure, easy manufacture and convenient disassembly, can rapidly generate a large amount of liquid sodium ferrate solution, and provides a set of feasible scheme for realizing the industrial preparation of the liquid sodium ferrate.
Drawings
FIG. 1 is a flow chart of the method of the present invention for producing liquid sodium ferrate based on an electrolytic process;
FIG. 2 is a front view of the electrolytic cell of the present invention;
FIG. 3 is a top view of the cell cover of the electrolytic cell of the present invention;
FIG. 4 is a left side view of the electrolytic cell of the present invention;
FIG. 5 is a left side view of the partition of the electrolytic cell of the present invention;
FIG. 6 is a right side view of the electrolytic cell of the present invention;
FIG. 7 is a graph showing the degradation of COD in petroleum wastewater by sodium ferrate in application example 1 of the present invention;
FIG. 8 is a graph showing the degradation of aniline in petroleum wastewater by sodium ferrate in application example 1 of the present invention;
FIG. 9 shows the reaction of sodium ferrate in application example 2 of the present invention on TCN in cyanide-containing wastewater－Degradation diagram of (2).
Detailed Description
In order to make the technical means and functions of the present invention easy to understand, the present invention is specifically described below with reference to the embodiments and the accompanying drawings.
The invention provides a method for preparing liquid sodium ferrate based on an electrolytic method, which is characterized by comprising the following steps:
And 2, adding the softened water into a stirrer containing a sodium hydroxide solution and a potassium chloride solution, stirring at a set speed, and uniformly mixing to prepare the electrolyte.
In the present invention, the concentration of the potassium chloride solution is 1 mol. L-1The concentration of the sodium hydroxide hydrolysate is 16 mol.L-1The stirring speed is 120 to 180 rad.min-1To ensure heat dissipation and mixingMixing uniformly.
And 3, adding the electrolyte into a condenser for condensation, and controlling the temperature to be 30-40 ℃ to obtain the condensed electrolyte.
Wherein, the sodium hydroxide is dissolved in water to release a large amount of heat, so the temperature of the electrolyte needs to be controlled to be 30-40 ℃ through the condenser 3.
And 4, adding the condensed electrolyte into an electrolytic cell, and electrolyzing the electrolyte for a certain time at a set current density to obtain a sodium ferrate solution.
In the invention, a constant-current and voltage-stabilized direct-current power supply is adopted, and the current density is 50mA/cm2～200mA/cm2The electrolysis duration is 1.5 h-3 h, and the current is reversed after every 0.5h of electrolysis for eliminating the passive film on the wire netting.
The invention also provides an electrolytic cell comprising: the groove comprises a groove body 1, three partition plates and four groove covers.
The tank body 1 is in a cuboid shape.
The partition plate 21, the partition plate 22, and the partition plate 23 are provided inside the tank body 1 to partition the tank body 1 into four regions, i.e., a first region 24, a second region 25, a third region 26, and a fourth region 27.
The slot cover 31, the slot cover 32, the slot cover 33 and the slot cover 34 are respectively arranged on the top of the slot body 1 and are used for covering the first area 24, the second area 25, the third area 26 and the fourth area 27.
In the invention, the lower parts of the four regions are communicated, the first region 24 is a liquid level height control region, the second region 25, the third region 26 and the fourth region 27 are electrolysis regions, each electrolysis region is provided with five pairs of grooves, each five pairs of grooves comprises three pairs of anode grooves and two pairs of cathode grooves, the number of the inserted electrode plates 12 is determined according to the requirement, and no diaphragm is arranged between the electrode plates 12.
In the invention, the tank body 1, the tank cover and the partition plate are all made of PP materials which are resistant to corrosion of alkaline liquid.
In the present invention, a liquid level sensor 4 is installed on the tank cover 31 of the first region 24, for automatically detecting the liquid level height,
the cover 32 of the second area 25, the cover 33 of the third area 26 and the cover 34 of the fourth area 27 are all provided with a fan 5 for removing hydrogen with reducibility generated in the electrolysis process.
As shown in fig. 4-6, number 6 is a sample inlet, 7 is a cathode tank, 8 is an anode tank, 9 is a pure nickel plate cathode, 10 is a wire mesh anode, and 11 is a water outlet.
In the invention, the anode material in the anode tank 8 is a wire mesh, the cathode material in the cathode tank 7 is a nickel plate, when electrolysis is carried out in the electrolytic tank, the current is required to be reversed every 0.5h for electrolysis, and the current is used for eliminating a passivation film on the wire mesh, namely, an oxidation film formed by passivation of the anode in the electrolysis process is damaged, so that the current efficiency is improved, and the energy consumption is reduced.
The electrode arrangement mode is as follows: the anode-cathode-anode arrangement mode is adopted, the anode material is common wire netting, the cathode material is a pure nickel plate, and the anode plate and the cathode plate are equal in size.
Measuring the concentration of sodium ferrate generated: detecting the absorbance of the sodium ferrate generated by electrolysis at the wavelength lambda of 510nm by using an ultraviolet spectrophotometer, and recording the absorbance value A, wherein the calculation formula is according to the beer-Lambert law formula: a ═ epsilon lc, where: ε is the absorptivity, and its value is 1150M-1cm-1L is the thickness of the cuvette, and c is the actual concentration of potassium ferrate.
< example 1>
16 mol. L-1Sodium hydroxide and 1 mol. L-1The potassium chloride mixed solution is taken as electrolyte, a wire mesh is taken as an anode, a pure nickel plate is taken as a cathode, the temperature of the electrolyte is controlled to be 35 ℃, and the current density is 50mA/cm2And the concentration of the potassium ferrate obtained after 3 hours of electrolysis is 33.37 mmol/L.
< example 2>
16 mol. L-1Sodium hydroxide and 1 mol. L-1The potassium chloride mixed solution is taken as electrolyte, a wire mesh is taken as an anode, a pure nickel plate is taken as a cathode, the temperature of the electrolyte is controlled to be 35 ℃, and the current density is 150mA/cm2And the concentration of the potassium ferrate obtained after 3 hours of electrolysis is 58.43 mmol/L.
< application example 1>
Along with the development of society, the demand of human beings on petroleum increases year by year, and oil fields adopt a 'secondary oil recovery' mode to recover oil on a large scale in order to improve the petroleum yield, so that the water content in crude oil produced liquid is continuously increased, a large amount of oily sewage is generated after oil-water separation, and how to treat the part of sewage becomes an important problem.
The sodium ferrate solution prepared in example 2 is used for carrying out degradation experiments on petroleum wastewater in a certain area of Chongqing according to different concentrations, the degradation effects on COD and aniline in the petroleum wastewater are researched, after the sodium ferrate solution reacts for 10min under different Fe (VI) concentrations, the COD and aniline change respectively as shown in figures 7 and 8, and the sodium ferrate solution can obviously degrade the COD and aniline, and the degradation rate is higher along with the increase of the sodium ferrate concentration, when the concentration of the sodium ferrate solution reaches 40mmol/L, the COD concentration is degraded from 78100ppm to 37800ppm, and the degradation rate is 51.6%; the aniline concentration is degraded from 20858ppm to 5249ppm, and the degradation rate is 74.8%.
< application example 2>
The sodium ferrate is safe and efficient for treating the low-concentration cyanide-containing electroplating wastewater, can solve the problems that the cyanide is not completely broken and the nickel hydroxide is easily oxidized into the nickelous hydroxide by the traditional sodium hypochlorite oxidation method, does not bring secondary pollution after treatment, and is a green treatment method. The sodium ferrate solution prepared in the example 2 is used for carrying out degradation experiments on electroplating wastewater in a certain area according to different concentrations, and TCN in the electroplating wastewater is researched-The degradation effect of (1) is that TCN is fully reacted under different Fe (VI) concentrations-The content change is shown in FIG. 9, and it can be seen that trace amount of sodium ferrate solution can be used for TCN-Has good degradation effect, and the concentration of the sodium ferrate solution is from 12 to 10-3The mmol/L is increased to 48X 10-3At mmol/L, the degradation rate is increased from 42% to nearly 100%.
Effects and effects of the embodiments
As is clear from application example 1 and FIGS. 7 and 8, when COD and aniline in liquid petroleum wastewater were degraded with a potassium ferrate solution having a concentration of 40mmol/L, the degradation rates were 51.6% and 74.8%, respectively. Therefore, the sodium ferrate solution can significantly degrade COD and aniline, and the degradation rate is higher as the concentration of sodium ferrate is increased.
As is clear from application example 2 and FIG. 9, the concentration of potassium ferrate used was from 12X 10-3The mmol/L is increased to 48X 10-3mmol/L of TCN in electroplating wastewater-When the degradation is carried out, the degradation rate is improved from 42 percent to nearly 100 percent. Thus, sodium ferrate solution versus TCN-Has good degradation effect, and the degradation rate is higher along with the increase of the concentration of the sodium ferrate, and the degradation rate is close to 100 percent.
The method for preparing liquid sodium ferrate based on the electrolytic method has the characteristics of simplicity, convenience, low raw material consumption, capability of degrading pollutants, good degradation effect, no secondary pollution and the like, and is more suitable for the technical processes of on-site preparation and addition.
In addition, the electrolytic cell has simple structure, easy manufacture and convenient disassembly, can rapidly generate a large amount of liquid sodium ferrate solution, and provides a set of feasible scheme for realizing the industrial preparation of the liquid sodium ferrate.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (7)
1. A method for preparing liquid sodium ferrate based on an electrolytic method is characterized by comprising the following steps:
step 1, softening water by using a softener to remove calcium, magnesium and other ions to obtain softened water;
step 2, adding the softened water into a stirrer with a sodium hydroxide solution and a potassium chloride solution, stirring at a set speed, and mixing uniformly to prepare an electrolyte;
step 3, adding the electrolyte into a condenser for condensation, and controlling the temperature to be 30-40 ℃ to obtain the condensed electrolyte;
and 4, adding the condensed electrolyte into an electrolytic cell, and electrolyzing the electrolyte for a certain time at a set current density to obtain a sodium ferrate solution.
2. The method for preparing liquid sodium ferrate based on the electrolytic method according to claim 1, wherein:
wherein, in the step 2, the concentration of the potassium chloride solution is 1 mol.L-1，
The concentration of the sodium hydroxide hydrolysate is 16 mol.L-1，
The stirring speed is 120 to 180 rad.min-1。
3. The method for preparing liquid sodium ferrate based on the electrolytic method according to claim 1, wherein:
wherein, in the step 4, the current density is 50mA/cm2～200mA/cm2，
The duration of electrolysis is 1.5-3 h.
4. An electrolytic cell for use in the method for producing liquid sodium ferrate based on the electrolytic process according to claim 1, for the electrolysis of an electrolyte, comprising:
the groove body is in a cuboid shape;
the three partition plates are arranged in the tank body and partition the tank body into four areas; and
four tank covers respectively placed at the top of the tank body for covering the four areas,
the lower parts of the four regions are communicated, the first region is a liquid level height control region, the second region, the third region and the fourth region are electrolysis regions, each electrolysis region is provided with five pairs of grooves, the five pairs of grooves comprise three pairs of anode grooves and two pairs of cathode grooves, the number of inserted electrode plates is determined according to needs, and no diaphragm is arranged between the electrode plates.
5. The electrolytic cell for implementing the method for the production of liquid sodium ferrate based on the electrolytic process according to claim 4, characterized in that:
the tank body, the tank cover and the partition plate are all made of PP materials resistant to corrosion of alkali liquor.
6. The electrolytic cell for implementing the method for the production of liquid sodium ferrate based on the electrolytic process according to claim 4, characterized in that:
wherein the tank cover of the first area is provided with a liquid level sensor for automatically detecting the liquid level height,
and the tank cover of the second area, the tank cover of the third area and the tank cover of the fourth area are respectively provided with a fan for removing reductive hydrogen generated in the electrolysis process.
7. The electrolytic cell for implementing the method for the production of liquid sodium ferrate based on the electrolytic process according to claim 4, characterized in that:
wherein the anode material in the anode tank is a wire mesh, the cathode material in the cathode tank is a nickel plate,
when electrolysis is carried out in the electrolytic cell, it is necessary to reverse the current for eliminating the passive film on the wire netting after every 0.5h of electrolysis.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090205973A1 (en) * | 2004-01-16 | 2009-08-20 | Monzyk Bruce F | Methods and apparatus for producing ferrate(vi) |
| US20110266159A1 (en) * | 2010-04-28 | 2011-11-03 | Osaka Electro-Communication University | Apparatus and method for producing electrolyzed water |
| CN106894037A (en) * | 2017-02-27 | 2017-06-27 | 东北电力大学 | A kind of method that electrolysis step by step produces high concentration ferrate |
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2020
- 2020-11-23 CN CN202011321170.1A patent/CN112746287A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090205973A1 (en) * | 2004-01-16 | 2009-08-20 | Monzyk Bruce F | Methods and apparatus for producing ferrate(vi) |
| US20110266159A1 (en) * | 2010-04-28 | 2011-11-03 | Osaka Electro-Communication University | Apparatus and method for producing electrolyzed water |
| CN106894037A (en) * | 2017-02-27 | 2017-06-27 | 东北电力大学 | A kind of method that electrolysis step by step produces high concentration ferrate |
Non-Patent Citations (1)
| Title |
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| 孙旭辉等: "电化学法制备高铁酸盐条件优化的研究", 《东北电力大学学报》 * |
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Application publication date: 20210504 |