CN101497461B - Method for rapidly preparing ferrate solution by microwave radiation - Google Patents
Method for rapidly preparing ferrate solution by microwave radiation Download PDFInfo
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- CN101497461B CN101497461B CN 200910064396 CN200910064396A CN101497461B CN 101497461 B CN101497461 B CN 101497461B CN 200910064396 CN200910064396 CN 200910064396 CN 200910064396 A CN200910064396 A CN 200910064396A CN 101497461 B CN101497461 B CN 101497461B
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- ferroferric oxide
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Abstract
The invention discloses a method for quickly preparing a ferrate solution by taking ferroferric oxide as an iron source under the microwave radiation condition. The method comprises that: firstly, a strong base solution is added into a reactor, ferroferric oxide powder is added into the reactor, and the mixture is heated and boiled until the solution is pasty; secondly, the mass ratio of the ferroferric oxide powder to the strong base solution is 1:2-6, and the concentration of the strong base solution is between 25 and 45 percent; thirdly, a NaClO solution with active chlorine of between 8 and 15 percent is added, the mass ratio of the ferroferric oxide powder to the NaClO solution is 1:2-8, and the mixture is heated under normal pressure for 0.5 to 5 minutes under the electromagnetic wave radiation condition; and fourthly, the ferrate solution can be obtained by centrifugation or filtration. The method opens up a new way for the preparation of ferrate, has the advantages of simple and convenient operation, quickness, energy conservation, and easy control, is applicable to production for immediate use, and solves the problems that the ferrate solution is difficult to preserve, and the like; and ferroferric oxide residue which does not react completely during the preparation can be taken as an iron source for recycle use after drying, so that the method saves the cost, is favorable for the environmental protection, and is easy for popularization.
Description
One, technical field:
The present invention relates to a kind of preparation method of compound, particularly relate to a kind of under the microwave radiation condition take the method for Z 250 as the source of iron rapid preparing ferrate solution.
Two, technical background:
Germany chemistry in 1702 and physicist Georg Stahl have found ferrate first.Research to ferrate starts from mid-term in 19th century.Fremy had synthesized potassium ferrate first in 1841, and Grory had delivered the article to the research of potassium ferrate purity check in 1893.In this a century, the research of ferrate is not greatly developed, until twentieth century forties, people just pay attention to again the research of ferrate.
Ferrate typically refers to potassium ferrate, Na2Fe04, and wherein iron is sexavalence, has very strong oxidisability, is applied to many fields by people at present.For example, potassium ferrate has sterilizing power by force, fast and do not produce the characteristics of the objectionable constituent such as trichloromethane when the disinfection of drinking water agent; Make magnetic memory material, make various types of hydrous iron oxides by controlling the potassium ferrate decomposition rate; When making electrode materials, have advantages of that specific storage is high, cycle life good.In recent years ferrate is permitted many-sided research as electrode materials and alkaline cell and lithium ion battery etc. also more.Yet the problems such as complicated and product stability is poor due to ferrate preparation, it is made slow progress aspect suitability for industrialized production at present.
Microwave technology is a newer subject, since people such as Aub-Samra after dissolving some biological samples with the microwave oven wet method first in 1975, microwave technology just with quick, efficient, energy-conservation, reduce the characteristics such as pollutions analyze and preparation in application more and more wider, there are food, environmental protection, medicine, metallurgy, nanotechnology etc. in the field that relates generally to.Microwave refers to the hertzian wave of frequency between 300～300000MHz.Microwave technology is one of method most characteristic in the novel material synthetic method, and the method has overcome all drawbacks of high temperature solid-state method, have fast, efficient, the characteristics such as be heated evenly, in recent years, utilize microwave heating technique to accelerate the existing many reports of chemical reaction.
Through retrieval, look into and mainly contain to the document of carry out microwave radiation heating application with ferrate technology of preparing and application thereof: Dong Jixi, " preparing the cobaltous phosphate nanoparticle with microwave radiation " of Zhang Wenmin, chemistry world, 1996,2:68～71; " the synthetic and physicochemical property research of ferric acid tripotassium sodium " of He Wei's spring, Wang Jianming etc., chemical journal, 2007 (20): 2261-2265; " the potassium ferrate Advances in Stability " of Pei Huixia, Li Fuxiang etc., Shanxi chemical industry, 2007 (4): 21-23; " the ferrate progress " of Zhang Xueying, Yang Changchun etc., synthetic chemistry, 2006 (2): 113-117; " Green Synthetic Oxidant Ferrate " of Song Hua, Wang Baohui, chemistry circular, 2003 (4) 242-257; Jiang Hongquan, " chemical oxidization method prepares the process for cleanly preparing of potassium ferrate " of Wang Peng etc., modern chemical industry, 2001,21 (6): 31-34; " preparation and application of Green Oxidant Ferrate " of Xia Qingyu, Fang Yi etc., chemical industry progress .2005,24 (3) .245-250; " the ferrate progress " of Zhang Xueying, Yang Changchun etc., synthetic chemistry .2006,14 (2) .-113-117; " the synthetic and performance of potassium ferrate " of Lu Chenghui, Li Jun etc., chemical research and application .2005,17 (4) .-495-497.
Relevant patent documentation has: number of patent application is 200510051369.6, and name is called the application documents of " divalence and the ferric iron mineral compound that are suitable for the electrosynthesis ferrate "; Number of patent application is 01106769.1, and name is called the application documents of " field preparation process for ferrate and system thereof "; Application number is 200610124990.5, and name is called the application documents of " a kind of method of utilizing iron and steel pickling waste liquid to prepare potassium ferrate "; The patent No. is 200310103164.9, and name is called the patent document of " method of rapid preparing ferrate solution ".
Do not see the report that carry out microwave radiation heating prepares ferrate in the above-mentioned document of consulting, have no the method for preparing ferrate solution take Z 250 as source of iron yet.The document of wherein wet chemical preparation is mostly take molysite such as iron(ic) chloride or iron nitrate as iron material, have individually take ironic hydroxide, ferrous sulfate as raw material.
Three, summary of the invention:
The technical problem to be solved in the present invention: a kind of method for preparing ferrate solution under the microwave radiation condition take Z 250 as source of iron is provided, and the method is easy and simple to handle, quick, but now-making-now-using.
Technical scheme of the present invention:
The present invention makes ferrate solution fast take Z 250 as source of iron under the microwave radiation condition.
Reaction principle is:
A kind of method of rapidly preparing ferrate solution by microwave radiation comprises the steps:
A. strong base solution is added reactor, drop into ferroferric oxide powder, heated and boiled; The mass ratio of described ferroferric oxide powder and strong base solution is 1: 2～6, and the strong base solution mass percent concentration is 25～45%;
B. adding available chlorine is 8～15% NaClO solution, reacts under electromagenetic wave radiation 0.5～5 minute, and the mass ratio of ferroferric oxide powder and NaClO solution is 1: 2～8;
C. can obtain ferrate solution through centrifugal or filtration.
Described highly basic is NaOH or KOH, and heated and boiled is that the reaction soln heated and boiled is to nearly pasty state; Wave frequency is 900MHz～3000MHz; Ferrate solution is atropurpureus solution.
In addition, also available molysite (as iron(ic) chloride, iron nitrate) or ferric oxide substitute the method Z 250 used.
Beneficial effect of the present invention:
Provided by the invention under the microwave radiation condition take the method for Z 250 as the source of iron rapid preparing ferrate solution, the concentration of prepared ferrate solution is not less than the ferrate concentration for preparing for source of iron with molysite (or ferric oxide) in other wet methods, and the method has been opened up a kind of new approach for the preparation ferrate.
2. the inventive method is easy and simple to handle, quick, and is energy-conservation, easy to control, is suitable for existing use and now makes, and avoided ferrate solution and has been difficult for the problems such as preservation, applies for ferrate good support is provided.
3. after the Z 250 residue drying that does not react completely in the inventive method, can recycle as source of iron, to save cost, be conducive to environment protection.
Four, embodiment:
Describe the present invention in detail below in conjunction with embodiment.
Embodiment 1:
Take ferroferric oxide powder 9.3g and put into that the 30ml mass percent is 32%, density is 1.35g/m
3NaOH solution in, stir evenly, heated and boiled is to the nearly pasty state of solution, then to add available chlorine be 11% NaClO solution 20ml, react 0.5～1.5min under the electromagenetic wave radiation condition of 2450MHz, get through centrifugal the atropurpureus ferrate solution that concentration is about 2.6g/L.
Embodiment 2:
Taking ferroferric oxide powder 9.3g, to put into 20ml, mass percent be in 32% NaOH solution, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 20ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 0.5～1.5min gets through centrifugal the atropurpureus ferrate solution that concentration is about 2.1g/L.
Embodiment 3:
Taking ferroferric oxide powder 9.3g, to put into 30ml, mass percent be in 32% NaOH solution, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 30ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 0.5～1.5min gets through centrifugal the ferrate solution that concentration is about 3.2g/L.
Embodiment 4:
Taking ferroferric oxide powder 9.3g, to put into 30ml, mass percent be in 32% NaOH solution, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 40ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 0.5～1.5min gets through centrifugal the atropurpureus ferrate solution that concentration is about 2.8g/L.
Embodiment 5:
Take in the NaOH solution that ferroferric oxide powder 9.3g puts into 40ml 32%, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 30ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 0.5～1.5min gets through centrifugal the atropurpureus ferrate solution that concentration is about 3g/L.
Embodiment 6:
Take in the NaOH solution that ferroferric oxide powder 18.6g puts into 60ml 32%, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 60ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 1.5～2.5min gets through centrifugal the atropurpureus ferrate solution that concentration is about 3.6g/L.
Embodiment 7:
Take in the NaOH solution that ferroferric oxide powder 18.6g puts into 60ml 45%, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 60ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 3～4min gets through centrifugal the atropurpureus ferrate solution that concentration is about 4g/L.
Embodiment 8:
Take in the NaOH solution that ferroferric oxide powder 18.6g puts into 60ml 32%, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 8% NaClO solution 60ml again, react 3～4min under the electromagenetic wave radiation condition of 2450MHz, get through centrifugal the atropurpureus ferrate solution that concentration is about 1.8g/L.
Embodiment 9:
Take in the NaOH solution that ferric oxide 18.2g puts into 60ml 32%, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 60ml again, react 1.5～2.5min under the electromagenetic wave radiation condition of 2450MHz, get through centrifugal the ferrate solution that concentration is about 3.3g/L.
Embodiment 10:
Take in the NaOH solution that iron(ic) chloride 16.2g puts into 30ml 32%, stir evenly, heated and boiled is to the nearly pasty state of solution, adding available chlorine is 11% NaClO solution 30ml again, under the electromagenetic wave radiation condition of 2450MHz, reaction 0.5～1.5min gets through centrifugal the ferrate solution that concentration is about 1.6g/L.
Claims (2)
1. the method for a rapidly preparing ferrate solution by microwave radiation, is characterized in that, comprises the steps:
A. strong base solution is added reactor, drop into ferroferric oxide powder, heated and boiled is to nearly pasty state; Described ferroferric oxide powder and strong base solution mass ratio are 1: 2～6, and strong base solution concentration is 25～45%; Described highly basic is NaOH or KOH;
B. adding available chlorine is 8～15% NaClO solution, reacts under electromagenetic wave radiation 0.5～5 minute; The mass ratio of ferroferric oxide powder and NaClO solution is 1: 2～8;
C. through centrifugal or filtration, can obtain ferrate solution.
2. the method for rapidly preparing ferrate solution by microwave radiation according to claim 1, it is characterized in that: described wave frequency is 900MHz～3000MHz.
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| CN101497461B true CN101497461B (en) | 2013-06-05 |
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| CN103771531B (en) * | 2014-01-22 | 2015-06-03 | 哈尔滨工业大学 | Method for efficiently preparing ferrate based on nascent interfacial activity |
| CN107487833B (en) * | 2017-09-22 | 2021-03-19 | 河海大学 | Method for controlling generation amount of disinfection by-product haloacetonitrile |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559917A (en) * | 2004-02-15 | 2005-01-05 | 云南大学 | Process of synthesizing high titanate and application as dehydrator for algas thereby |
| CN1749166A (en) * | 2005-11-03 | 2006-03-22 | 深圳职业技术学院 | Process for preparing solid potassium ferrate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559917A (en) * | 2004-02-15 | 2005-01-05 | 云南大学 | Process of synthesizing high titanate and application as dehydrator for algas thereby |
| CN1749166A (en) * | 2005-11-03 | 2006-03-22 | 深圳职业技术学院 | Process for preparing solid potassium ferrate |
Non-Patent Citations (3)
| Title |
|---|
| Ji Yafei et al..Preparation of Potassium Ferrate(Ⅵ) via β-Fe2O3.Journal of China University of Mining & Technology.1999,9(1),22-24. |
| Ji Yafei et al..Preparation of Potassium Ferrate(Ⅵ) via β-Fe2O3.Journal of China University of Mining & * |
| Technology.1999,9(1),22-24. * |
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