CN103449527A - Method for preparing ferrate through hydraulic power cavitation and activation - Google Patents
Method for preparing ferrate through hydraulic power cavitation and activation Download PDFInfo
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- CN103449527A CN103449527A CN2013103536656A CN201310353665A CN103449527A CN 103449527 A CN103449527 A CN 103449527A CN 2013103536656 A CN2013103536656 A CN 2013103536656A CN 201310353665 A CN201310353665 A CN 201310353665A CN 103449527 A CN103449527 A CN 103449527A
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- hypochlorite
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Abstract
The invention relates to a method for preparing ferrate through hydraulic power cavitation and activation. The invention provides a preparation method of a water treatment agent, which can be used for preparation of a high-efficiency water treatment agent ferrate and belongs to the technical field of environmental protection. The method comprises the following steps: under the condition of sufficient stirring, adding an iron salt solution into a strongly alkaline solution, thus generating iron hydroxide; under the condition of sufficient stirring, adding a right amount of stabilizer, adding a hypochlorite solution, adding strong alkali solid powder until the powder is dissolved to saturation, performing cavitation treatment on the reaction materials through a hydraulic power cavitation reactor, and ensuring that Fe(OH)3 is sufficiently oxidized, thus generating a ferrate product; and cooling the solution, performing solid-liquid separation, purifying the ferrate in the solid phase to obtain the ferrate product, and recovering and returning the alkaline solution of the liquid phase. The method has the characteristics of low cost, high yield, high product purity, less equipment investment and the like, and is very suitable for preparation of ferrate.
Description
[technical field]
The present invention relates to a kind of method of preparation of water conditioner, can be used for the preparation of High-efficient Water treatment agent ferrate, belong to environmental technology field.
[background technology]
Ferrate refers to and contains Fe (VI) O
4the salt that acid group and metal ion form, it possesses very strong oxidisability, and its redox potential is 2.20V under acidic conditions, under alkaline condition, is 0.72V, compares KMnO
4, O
3, C1
2the oxygenant of relatively commonly using Deng these also is eager to excel.New and effective disinfection of drinking water agent and water conditioner as a kind of non-chlorine, it can be removed traditional water conditioner and be difficult to thoroughly remove harmful chloro pollutent, especially phenol and sulfide are had to obvious oxidation removal effect, the CN in oxidizing water safely and effectively
-.Except thering is extremely strong oxidisability, generate the Fe with height adsorption activity after reaction
3+, most of ion, organism and suspended substance can flocculate at very wide pH value scope internal adsorption.Potassium ferrate integrates oxidation, sterilization, absorption, it is solidifying to flocculate, help, decolouring, deodorizing etc. are multi-functional, and final product is nontoxic ferric ion, can not produce induced gene sudden change and carcinogenic effect, is eco-friendly treatment agent.Ferrate not only can be used as water conditioner, but also at aspects such as electrode active material, petrochemical catalysts, a lot of application is arranged, and therefore, the preparation method of research ferrate has become an important problem.
The preparation method of existing ferrate mainly contains three kinds of high temperature peroxide oxidation method, electrolytic process and hypochlorite methods.High temperature peroxide oxidation method is that the metal oxide with oxidisability is reacted to the ferrate method that generates with the oxide compound of iron, molysite or iron under the heat condition, this method needs strict red-tape operati condition, production cost is high, more dangerous and certainly be difficult to realize the there be limited evidence currently of employing.Electrolytic process is that oxidizing reaction occurs on iron anode. make iron or iron ion be oxidized to the method for high ferro acid group, this method exists the problems such as energy consumption is high, byproduct is more to have to be solved.Hypochlorite method is in the strong alkali solution environment, take saturated hypochlorite solutions and molysite as raw material, by hypochlorite, the oxidizing reaction of iron is generated the method for ferrate, this method mature production technology, facility investment is less, easily realizing, is a kind of preparation method commonly used, but because its oxidising process efficiency is lower, need to add excessive oxygenant, the cost that this not only increases, accelerated equipment corrosion, but also the difficulty of the product purification process strengthened.Therefore, strengthening its oxidising process, promote its oxidation efficiency, is that the reduction hypochlorite method prepares the cost of ferrate, an important channel of improving product quality.
[summary of the invention]
Purpose of the present invention is exactly to strengthen the oxidising process of hypochlorite by Hydrodynamic cavitation, improves oxidation efficiency, effectively solves the defect of above-mentioned alkali hypochlorite method.Existing hypochlorite method is that hypochlorite and molysite are added in strong alkali solution, and molysite first generates ferric hydroxide precipitate, and then by the hypochlorite oxidation.Its chemical reaction is:
Fe
3++3OH
-=Fe(OH)
3↓
2Fe(OH)
3+3C1O
-+4OH
-=2FeO
4 2-+5H
2O+3C1
-
Because oxidizing reaction occurs in the ironic hydroxide solid surface, this liquid and solid phase reaction process is easy to restriction, solid state reaction surface due to the liquid-solid phase mass transfer process and former the obstruction such as is passivated, and reaction efficiency is reduced.
If now material is carried out to cavitation process by cavitation reactor, the cavatition that Hydrodynamic cavitation produces can produce local high speed micro jet flow, the ironic hydroxide solid surface issues life-stylize in the impact of this high speed micro jet flow, on the solid surface of this activation, the oxidation reaction process of solid liquid phase is accelerated, on the other hand, micro jet flow has also accelerated the mass transfer process of solid-liquid phase reaction, therefore, no matter be that reaction is controlled or the solid liquid phase oxidising process of diffusion control, under cavatition, its reaction all is accelerated, and reaction efficiency is improved.
Therefore present method can be divided into following steps:
1, under well-beaten condition, iron salt solutions is added in strong alkali solution, generate ironic hydroxide.
2, under well-beaten condition, first add appropriate stablizer, then add hypochlorite solutions, finally supplementing the highly basic pressed powder, that it is dissolved to is saturated.
3, reaction mass is carried out to cavitation process by the Hydrodynamic cavitation reactor, allow Fe (OH)
3by fully oxidation, generate the ferrate product.
4, cooling, solid-liquid separation, carry out purifying by the ferrate generated in solid phase, obtains the ferrate product, the recycle of alkali liquor of liquid phase reuse.
The characteristics such as present method has low cost, high yield, product purity is high, facility investment is little, be well suited for the preparation of ferrate.
[embodiment]
Further illustrate the specific embodiment of the present invention and effect with following indefiniteness embodiment:
Embodiment 1
1, in the reactor of 1000 liters, add 120 liters of saturated potassium hydroxide solutions, under well-beaten condition, add gradually 60 liters of 45% liquor ferri trichloridis, more fully stir half an hour.
2, under well-beaten condition, first add 5 liters of 50% Cupric Chloride Solutions, then add 200 liters of potassium hypochlorite 3, the solution of 10% (available chlorine), finally add granularity to be less than 300 kilograms, 600 purpose potassium hydroxide powder, then stir half an hour.
3, reaction mass is inputted to the Hydrodynamic cavitation reactor repeatedly and carry out cavitation process, the Hydrodynamic cavitation reactor adopts venturi arrangement, controlling inlet feed pressure is 0.90Mpa, and top hole pressure is 0.15Mpa, and the accumulated process time of slurry in cavitation reactor reaches one hour.After cavitation process completes, it is transparent that solution is.
4, cooling solution to 0 ℃, the centrifugal solid phase that obtains is the thick product of potassium ferrate, the liquid phase recycle of alkali liquor is also reused.Saturated potassium hydroxide solution washing 5 times for thick product, washings is cooling, can also obtain potassium ferrate solid.By reaching the cooling potassium ferrate solid obtained of washings after washing successively with methyl alcohol, ether washing, can obtain pure potassium ferrate product after suction filtration, drying.
Prepare potassium ferrate according to above-mentioned steps, yield reaches 91.2%, and product purity reaches 98.3%.
Embodiment 2
1, in the reactor of 1000 liters, add 120 liters of saturated sodium hydroxide solutions, at audio frequency, be under 22kHz, the power Ultrasonic Radiation that is 1.2kw, well-beaten condition, add gradually 100 liters of saturated iron nitrate solutions, more fully stir 40 minutes.
2, under well-beaten condition, first add 15 liters of 15% sodium silicate solutions, then add 150 liters of the chlorine bleach liquores of 10% (available chlorine), finally add granularity to be less than 300 kilograms of 600 purpose sodium hydroxide powder, then stir half an hour.
3, reaction mass is inputted to the Hydrodynamic cavitation reactor repeatedly and carry out cavitation process, the Hydrodynamic cavitation reactor adopts liquid whistle device, controlling cavitation reactor inlet feed pressure is 0.85Mpa, and top hole pressure is 0.15Mpa, and the accumulated process time of reaction mass in cavitation reactor reaches 1.5 hours.After cavitation process completes, it is transparent that solution is.
4, cooling solution to 0 ℃, the centrifugal thick product of Na2Fe04 that obtains, then wash 5 times with saturated sodium hydroxide solution, washings is cooling, can obtain the Na2Fe04 solid.By reaching the cooling Na2Fe04 solid obtained of washings after washing successively with methyl alcohol, ether washing, can obtain pure Na2Fe04 product after the suction filtration drying.
Prepare Na2Fe04 according to above-mentioned steps, yield reaches 89.8%, and product purity reaches 97.8%.
Embodiment 3
1, in the reactor of 1000 liters, add 100 liters of saturated potassium hydroxide solutions, at audio frequency, be under 25kHz, the power Ultrasonic Radiation that is 1.5kw, well-beaten condition, add gradually 100 liters of saturated iron nitrate solutions, more fully stir half an hour.
2, under well-beaten condition, add successively 5 liters of 15% sodium silicate solutions, 2 liters of 50 Cupric Chloride Solutions, 200 liters of the chlorine bleach liquores of 10% (available chlorine), finally add granularity to be less than 350 kilograms, 600 purpose potassium hydroxide powder, then stir half an hour.
3, reaction mass is inputted to the Hydrodynamic cavitation reactor repeatedly and carry out cavitation process, the Hydrodynamic cavitation reactor adopts the porous plate device, porous plate aperture 2.5mm, thickness of slab 10mm, the ratio 0.125 that hole area is long-pending with the cavitation reactor cross-section of pipeline, cavitation reactor inlet feed pressure is 0.75Mpa, and top hole pressure is 0.15Mpa, and the control accumulated process time of slurry in cavitation reactor reaches 2 hours.After cavitation process completes, it is transparent that solution is.
4, cooling solution to 0 ℃, the centrifugal thick product of potassium ferrate that obtains, then wash 5 times with saturated potassium hydroxide solution, washings is cooling, can obtain potassium ferrate solid.By reaching the cooling potassium ferrate solid obtained of washings after washing successively with methyl alcohol, ether washing, can obtain pure potassium ferrate product after the suction filtration drying.
Prepare potassium ferrate according to above-mentioned steps, yield reaches 90.1%, and product purity reaches 96.3%.
Above-described embodiment has only expressed the preferred embodiment of the present invention, can not be interpreted as the restriction to the scope of the claims of the present invention, so the present invention is not limited to this concrete technical process.Those skilled in the art, according to technical scheme of the present invention and design, can also make some distortion and improvement, and these all belong to protection scope of the present invention.So all other embodiments that draw according to the claims in the present invention scope, all should belong to the scope that the present invention is contained.
Claims (6)
1. a Hydrodynamic cavitation activates the method for preparing ferrate, it is characterized in that comprising following steps:
(1), under well-beaten condition, iron salt solutions is added in strong alkali solution, generate ironic hydroxide.
(2), under well-beaten condition, first add appropriate stablizer, then add hypochlorite solutions, finally supplementing the highly basic pressed powder, that it is dissolved to is saturated.
(3) reaction mass is carried out to cavitation process by the Hydrodynamic cavitation reactor, allow Fe (OH)
3by fully oxidation, generate the ferrate product.
(4), cooling, solid-liquid separation, carry out purifying by the ferrate generated in solid phase, obtains the ferrate product, the recycle of alkali liquor of liquid phase reuse.
2. preparation method according to claim 1 is characterized in that: described Hydrodynamic cavitation reactor is a kind of in orifice plate, Venturi tube, the liquid whistle.
3. preparation method according to claim 1 is characterized in that: described highly basic is a kind of in potassium hydroxide or sodium hydroxide.
4. preparation method according to claim 1 is characterized in that: the molysite of described (1) step is a kind of in iron(ic) chloride or iron nitrate.
5. preparation method according to claim 1 is characterized in that: the hypochlorite of described (2) step is a kind of in clorox or potassium hypochlorite.
6. preparation method according to claim 1, it is characterized in that: the stablizer of described (2) step is a kind of or or its mixture in cupric chloride, water glass.
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Cited By (9)
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WO2015110050A1 (en) * | 2014-01-22 | 2015-07-30 | 哈尔滨工业大学 | Method for efficiently preparing ferrate based on nascent interfacial activity |
CN104828885A (en) * | 2015-05-18 | 2015-08-12 | 陈雷 | Preparation method of liquid ferrate |
CN104828920A (en) * | 2015-05-18 | 2015-08-12 | 陈雷 | Preparation method of poly ferric perchloride flocculant |
CN105923735A (en) * | 2016-06-02 | 2016-09-07 | 南京大学 | Compound water treatment agent based on ferrate and preparation method of compound water treatment agent |
CN106745300A (en) * | 2017-01-20 | 2017-05-31 | 福建师范大学福清分校 | The high efficiency preparation method of ferrate |
CN107138738A (en) * | 2017-05-23 | 2017-09-08 | 天津工业大学 | A kind of method and device of Fast back-projection algorithm silver nano-grain |
CN107175339A (en) * | 2017-05-23 | 2017-09-19 | 天津工业大学 | A kind of method and device without reducing agent Fast back-projection algorithm gold nano grain |
CN108751380A (en) * | 2018-06-19 | 2018-11-06 | 怀化学院 | A kind of processing method of phase chromatography-use methanol waste water |
CN115394467A (en) * | 2022-09-05 | 2022-11-25 | 哈尔滨工业大学 | Method for treating aluminosilicate in nuclear waste by using cavitation activation water |
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CN102026718A (en) * | 2008-05-15 | 2011-04-20 | 希卡技术私人有限公司 | Method of designing hydrodynamic cavitation reactors for process intensification |
CN103145189A (en) * | 2013-03-01 | 2013-06-12 | 凤台精兴生物科技有限公司 | Preparation method of potassium ferrate |
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US5746994A (en) * | 1996-08-09 | 1998-05-05 | New Mexico State University Technology Transfer Corporation | Method for synthesizing ferrate and ferrate produced thereby |
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015110050A1 (en) * | 2014-01-22 | 2015-07-30 | 哈尔滨工业大学 | Method for efficiently preparing ferrate based on nascent interfacial activity |
WO2015109683A1 (en) * | 2014-01-22 | 2015-07-30 | 哈尔滨工业大学 | Method for efficiently preparing ferrate based on nascent interfacial activity |
CN104828885A (en) * | 2015-05-18 | 2015-08-12 | 陈雷 | Preparation method of liquid ferrate |
CN104828920A (en) * | 2015-05-18 | 2015-08-12 | 陈雷 | Preparation method of poly ferric perchloride flocculant |
CN105923735A (en) * | 2016-06-02 | 2016-09-07 | 南京大学 | Compound water treatment agent based on ferrate and preparation method of compound water treatment agent |
CN105923735B (en) * | 2016-06-02 | 2018-11-13 | 南京大学 | A kind of composite water treatment medicament and preparation method thereof based on ferrate |
CN106745300A (en) * | 2017-01-20 | 2017-05-31 | 福建师范大学福清分校 | The high efficiency preparation method of ferrate |
CN107138738A (en) * | 2017-05-23 | 2017-09-08 | 天津工业大学 | A kind of method and device of Fast back-projection algorithm silver nano-grain |
CN107175339A (en) * | 2017-05-23 | 2017-09-19 | 天津工业大学 | A kind of method and device without reducing agent Fast back-projection algorithm gold nano grain |
CN108751380A (en) * | 2018-06-19 | 2018-11-06 | 怀化学院 | A kind of processing method of phase chromatography-use methanol waste water |
CN115394467A (en) * | 2022-09-05 | 2022-11-25 | 哈尔滨工业大学 | Method for treating aluminosilicate in nuclear waste by using cavitation activation water |
CN115394467B (en) * | 2022-09-05 | 2023-04-28 | 哈尔滨工业大学 | Method for treating aluminosilicate in nuclear waste by cavitation activated water |
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Application publication date: 20131218 |