CN104261481B - Preparation method of potassium ferrate - Google Patents
Preparation method of potassium ferrate Download PDFInfo
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Abstract
The invention discloses a preparation method of a potassium ferrate solid, belonging to the technical field of water treatment. The preparation method comprises the following steps: (1) preparing alkaline saturated potassium hypochlorite solution by reacting calcium hypochlorite with potassium carbonate; (2) in an ice-water bath environment, adding ferric nitrate nonahydrate solid into an alkaline saturated potassium hypochlorite solution to generate a potassium ferrate solution; (3) adding saturated potassium hydroxide solution into potassium ferrate solution, standing in ice water bath, and performing suction filtration to obtain a crude solid potassium ferrate product; (4) dissolving the crude potassium ferrate product by using a potassium hydroxide solution, carrying out suction filtration, recrystallizing in an ice-water bath, and carrying out suction filtration to obtain a recrystallized potassium ferrate solid; (5) sequentially leaching and recrystallizing the potassium ferrate solid by using normal hexane, ethanol, normal pentane and ethanol, and drying the potassium ferrate solid in vacuum to constant weight to obtain the finished product of the potassium ferrate powder solid. The method is simple to operate, avoids the use of hazardous gases such as chlorine and ether, is high in safety, and the prepared potassium ferrate is high in purity (> 98%).
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of preparation method of safe and simple water treatment potassium ferrate solid.
Background technology
Potassium ferrate is a kind of sexavalence molysite, has strong oxidizing property, is that one integrates the functions such as oxidation, flocculation, absorption, sterilization, and does not produce the Green Water Treatment Reagents of the objectionable impuritiess such as haloform after reaction, has great application prospect.
At present, the preparation method of potassium ferrate is mainly divided into three major types: superoxide high-temperature oxidation, electrochemical process, hypochlorite oxidation method.Wherein, under alkaline condition, it is that a kind of use is maximum that hypochlorite oxidation's trivalent iron salt prepares potassium ferrate, the method for relative maturity.Nineteen fifty Hrostowski and scott proposes two-step approach and prepares potassium ferrate, namely first in the basic conditions, hypochlorite oxidation iron trichloride can obtain Na2Fe04, and then utilize the solubleness of potassium ferrate under basic conditions to be less than the feature of Na2Fe04, Na2Fe04 is changed into potassium ferrate.The method is carried out in two steps, complicated operation, productive rate lower (being no more than 10%).In order to simplify the operation, chlorine is passed into the saturated potassium hypochlorite of preparation alkalescence in potassium hydroxide solution and carrys out direct oxidation trivalent iron salt by Jiang Hongquans etc., realize a step directly to prepare potassium ferrate (chemical oxidization method prepares the process for cleanly preparing [J] of potassium ferrate, modern chemical industry, 2001,21 (6): 31-34.).Current many disclosed patent (CN1749166A, CN101597087A, CN100532261C, CN101117240A, CN102701286A, CN103265084A) mostly adopt the method for alkali liquor absorption chlorine to prepare potassium hypochlorite for being oxidized ferric iron generation potassium ferrate.Owing to using in process of production, there is toxicity and corrosive hazardous gas chlorine, therefore require higher to the resistance to air loss of production unit and erosion resistance, easily cause security incident.In addition, in the process, excessive alkali need be added, the Repone K of generation is separated out from potassium hypochlorite solution, in order to avoid affect the purity of follow-up ferrate, but this process wastes too much alkali lye on the one hand, on the other hand, Repone K is separated out not exclusively from potassium hypochlorite solution, makes the purification process more complicated of follow-up potassium ferrate.The trial Losantin such as Zhou Weiwei replaces chlorine and potassium hydroxide to react preparing the potassium hypochlorite (preparation of potassium ferrate and remove the research [J] of dihydroxyphenyl propane ability in micro-polluted water, water technology, 2013,39 (10): 72-75.), but this process generates the calcium hydroxide of microsolubility, and it still can not separate completely preferably in potassium hypochlorite solution.
Summary of the invention
For the above technical problem that prior art exists, produce the potential potential safety hazard brought to ferrate in order to avoid chlorine uses, simplify preparation process and improve product purity further, the invention provides a kind of safe and simple potassium ferrate preparation method, namely potassium hypochlorite solution is prepared with Losantin and salt of wormwood reaction, add nine water iron nitrate powder, react under ice-water bath condition, prepare highly purified potassium ferrate solid.
The concrete steps of a kind of safe and simple potassium ferrate preparation method provided by the present invention are as follows:
(1) ratio of 1.5:1 in mass ratio, take Losantin and salt of wormwood respectively, and be configured to equal-volume solution, both mixing, after reaction 15min, cross and filter precipitation of calcium carbonate, filtrate is placed in ice-water bath, limit is stirred, while slowly add potassium hydroxide solid (carrying out according to the ratio adding 1g potassium hydroxide solid in every milliliter of filtrate) in filtrate, obtains alkaline saturated potassium hypochlorite solution;
(2) in ice water bath environment, nine water iron nitrate solids (add-on is 3.9 times of salt of wormwood quality in step (1)) are slowly added in the saturated potassium hypochlorite solution of alkalescence prepared by step (1), stir with the rotating speed of 900r/min, after reaction 60min, generate potassium ferrate solution;
(3) in the potassium ferrate solution prepared by step (2), add the saturated potassium hydroxide solution of equal-volume, after leaving standstill 30min in ice water bath environment, with G2 glass sand core funnel suction filtration, obtain the thick product of potassium ferrate solid;
(4) with 3mo/L potassium hydroxide solution (consumption is according to the proportionlity of every 1g potassium ferrate thick product 25ml potassium hydroxide solution) the thick product of potassium ferrate prepared by dissolving step (3), with G3 glass sand core funnel suction filtration, saturated potassium hydroxide solution is added in filtrate, add-on is 4 times of above-mentioned 3mo/L potassium hydroxide solution volume, recrystallization 40min is stirred in ice water bath environment, with G3 glass sand core funnel suction filtration, obtain potassium ferrate solid after recrystallization;
(5) after priority normal hexane, ethanol, Skellysolve A, ethanol embathe the recrystallization that step (4) obtains, (normal hexane, Skellysolve A consumption use according to the ratio of potassium ferrate 20ml after 1g recrystallization potassium ferrate solid respectively, ethanol consumption uses according to the ratio of potassium ferrate 5ml after 1g recrystallization respectively), after at 60 DEG C of temperature, vacuum-drying is to constant weight, obtain finished product potassium ferrate powder solid, sealing, preserves.
The principles of science of the present invention:
The principles of science of the present invention is mainly based on following two chemical equation:
Ca(ClO)
2+K
2CO
3＝CaCO
3↓+2KClO(1)
2Fe(NO
3)
3+3KClO+10KOH＝2K
2FeO
4+6KNO
3+3KCl+5H
2O(2)
First take appropriate Losantin according to reaction formula (1) and salt of wormwood is mixed with solution, hybrid reaction, filter and remove precipitation of calcium carbonate, filtrate is yellowish green potassium hypochlorite solution.Then the iron nitrate of grind into powder is joined in potassium hypochlorite solution, under strongly alkaline conditions, prepare potassium ferrate according to formula (2) reaction.
Compared with prior art, the present invention has the following advantages:
1) the present invention is with Ca (ClO)
2and K
2cO
3potassium hypochlorite solution is prepared in reaction, avoid the use with toxicity and corrosive chlorine, eliminate potential safety hazard that hazardous gas chlorine brings production process, do not need resistance to air loss and erosion resistance to require higher production unit, production process is simplified, controllability is good, and safety coefficient increases substantially.
2) the present invention is with Ca (ClO)
2and K
2cO
3reaction prepares potassium hypochlorite solution, the CaCO generated in reaction
3precipitation solubility is little, is easy to filter remove, and decrease the use of alkali lye, in potassium hypochlorite solution, impurity is less, and the oxidation efficiency of follow-up potassium ferrate improves, and impurity is few, simplifies subsequent purification steps, and product purity and productive rate are improved.
3) the present invention is used alternatingly normal hexane, ethanol, Skellysolve A, ethanol mode dewater to ferrate solid after crystallization, removal of impurity salt, avoids the use of toxic and harmful ether, improves the security of product purity and production process.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the preparation-obtained potassium ferrate solid of the embodiment of the present invention 1;
As can be seen from the figure: prepared product is at 809.54cm
-1there is obviously sharp-pointed absorption peak at place, shows that this product is potassium ferrate.
Fig. 2 is the UV-vis spectroscopy spectral scan figure of the preparation-obtained potassium ferrate liquid of the embodiment of the present invention 1;
As can be seen from the figure: the solution of prepared product has potassium ferrate charateristic avsorption band at 505nm place, prove that this sample is potassium ferrate really.
Embodiment
Below in conjunction with specific embodiment in detail the present invention is described in detail, but the present invention is not limited to following embodiment.
Embodiment 1
(1) Losantin 8.00g and salt of wormwood 5.33g is taken respectively, and be configured to each 50ml of equal-volume solution, both mixing, after reaction 15min, cross and filter precipitation of calcium carbonate, filtrate is placed in ice-water bath, limit is stirred, while slowly add potassium hydroxide solid 100g in filtrate, obtain alkaline saturated potassium hypochlorite solution;
(2) in ice water bath environment, in the saturated potassium hypochlorite solution of alkalescence prepared by step (1), slowly add nine water iron nitrate solid 20.79g, stir with the rotating speed of 900r/min, after reaction 60min, generate potassium ferrate solution;
(3) in the potassium ferrate solution prepared by step (2), add the saturated potassium hydroxide solution of 100ml, after leaving standstill 30min in ice water bath environment, with G2 glass sand core funnel suction filtration, obtain the thick product of potassium ferrate solid;
(4) with the thick product of potassium ferrate prepared by 3mo/L potassium hydroxide solution 45ml dissolving step (3), with G3 glass sand core funnel suction filtration, saturated potassium hydroxide solution 180ml is added in filtrate, add-on is 4 times of above-mentioned 3mo/L potassium hydroxide solution volume, recrystallization 40min is stirred in ice water bath environment, with G3 glass sand core funnel suction filtration, obtain potassium ferrate solid after recrystallization;
(5) priority normal hexane 36ml, ethanol 9ml, Skellysolve A 36ml, ethanol 9ml embathe potassium ferrate solid after the recrystallization that step (4) obtains, after at 60 DEG C of temperature, vacuum-drying, to constant weight, obtains finished product potassium ferrate powder solid, sealing, preserves.
Embodiment 2
(1) Losantin 12.00g and salt of wormwood 8.00g is taken respectively, and be configured to each 100ml of equal-volume solution, both mixing, after reaction 15min, cross and filter precipitation of calcium carbonate, filtrate is placed in ice-water bath, limit is stirred, while slowly add potassium hydroxide solid 200g in filtrate, obtain alkaline saturated potassium hypochlorite solution;
(2) in ice water bath environment, in the saturated potassium hypochlorite solution of alkalescence prepared by step (1), slowly add nine water iron nitrate solid 31.20g, stir with the rotating speed of 900r/min, after reaction 60min, generate potassium ferrate solution;
(3) in the potassium ferrate solution prepared by step (2), add the saturated potassium hydroxide solution of 200ml, after leaving standstill 30min in ice water bath environment, with G2 glass sand core funnel suction filtration, obtain the thick product of potassium ferrate solid;
(4) with the thick product of potassium ferrate prepared by 3mo/L potassium hydroxide solution 75ml dissolving step (3), with G3 glass sand core funnel suction filtration, saturated potassium hydroxide solution 300ml is added in filtrate, add-on is 4 times of above-mentioned 3mo/L potassium hydroxide solution volume, recrystallization 40min is stirred in ice water bath environment, with G3 glass sand core funnel suction filtration, obtain potassium ferrate solid after recrystallization;
(5) priority normal hexane 60ml, ethanol 15ml, Skellysolve A 60ml, ethanol 15ml embathe potassium ferrate solid after the recrystallization that step (4) obtains, after at 60 DEG C of temperature, vacuum-drying, to constant weight, obtains finished product potassium ferrate powder solid, sealing, preserves.
Embodiment 3
(1) Losantin 18.00g and salt of wormwood 12.00g is taken respectively, and be configured to each 100ml of equal-volume solution, both mixing, after reaction 15min, cross and filter precipitation of calcium carbonate, filtrate is placed in ice-water bath, limit is stirred, while slowly add potassium hydroxide solid 200g in filtrate, obtain alkaline saturated potassium hypochlorite solution;
(2) in ice water bath environment, in the saturated potassium hypochlorite solution of alkalescence prepared by step (1), slowly add nine water iron nitrate solid 46.80g, stir with the rotating speed of 900r/min, after reaction 60min, generate potassium ferrate solution;
(3) in the potassium ferrate solution prepared by step (2), add the saturated potassium hydroxide solution of 200ml, after leaving standstill 30min in ice water bath environment, with G2 glass sand core funnel suction filtration, obtain the thick product of potassium ferrate solid;
(4) with the thick product of potassium ferrate prepared by 3mo/L potassium hydroxide solution 100ml dissolving step (3), with G3 glass sand core funnel suction filtration, saturated potassium hydroxide solution 400ml is added in filtrate, add-on is 4 times of above-mentioned 3mo/L potassium hydroxide solution volume, recrystallization 40min is stirred in ice water bath environment, with G3 glass sand core funnel suction filtration, obtain potassium ferrate solid after recrystallization;
(5) priority normal hexane 81ml, ethanol 20ml, Skellysolve A 81ml, ethanol 20ml embathe potassium ferrate solid after the recrystallization that step (4) obtains, after at 60 DEG C of temperature, vacuum-drying, to constant weight, obtains finished product potassium ferrate powder solid, sealing, preserves.
Take the potassium ferrate sample prepared by a certain amount of above-described embodiment 1 ~ 3, be dissolved in respectively in the distilled water of certain volume, in acid condition Fe
6+resolve into Fe
3+, add oxammonium hydrochloride by Fe
3+be reduced to Fe further
2+, adopt Fe in spectrophotometric determination o-phenanthroline water
2+content, according to the ferro element mass conservation, the content of indirect calculation potassium ferrate, calculates the purity of prepared potassium ferrate then.Known through aforesaid method quantitative analysis, the potassium ferrate purity prepared by three kinds of embodiments is all more than 98.70%.
Claims (1)
1. a preparation method for potassium ferrate, is characterized in that, these preparation method's concrete steps are as follows:
(1) ratio of 1.5:1 in mass ratio, take Losantin and salt of wormwood respectively, and be configured to equal-volume solution, both mixing, after reaction 15min, cross and filter precipitation of calcium carbonate, filtrate is placed in ice-water bath, and according to the ratio adding 1g potassium hydroxide solid in every milliliter of filtrate, filtrate is stirred on limit, limit slowly adds potassium hydroxide solid wherein, obtains alkaline saturated potassium hypochlorite solution;
(2) in ice water bath environment, in the saturated potassium hypochlorite solution of alkalescence prepared by step (1), slowly add nine water iron nitrate solids, stir with the rotating speed of 900r/min, after reaction 60min, generate potassium ferrate solution; Described nine water iron nitrate solids loading content are 3.9 times of salt of wormwood quality in step (1);
(3) in the potassium ferrate solution prepared by step (2), add the saturated potassium hydroxide solution of equal-volume, after leaving standstill 30min in ice water bath environment, with G2 glass sand core funnel suction filtration, obtain the thick product of potassium ferrate solid;
(4) according to the ratio of every 1g potassium ferrate thick product 25ml potassium hydroxide solution, with the thick product of potassium ferrate prepared by 3mo/L potassium hydroxide solution dissolving step (3), with G3 glass sand core funnel suction filtration, saturated potassium hydroxide solution is added in filtrate, add-on is 4 times of above-mentioned 3mo/L potassium hydroxide solution volume, stir recrystallization 40min in ice water bath environment, with G3 glass sand core funnel suction filtration, obtain potassium ferrate solid after recrystallization;
(5) priority normal hexane, ethanol, Skellysolve A, ethanol embathe potassium ferrate solid after the recrystallization that step (4) obtains, after at 60 DEG C of temperature, vacuum-drying, to constant weight, obtains finished product potassium ferrate powder solid.
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| CN108046332A (en) * | 2018-01-26 | 2018-05-18 | 哈尔滨工业大学 | The preparation method of high-valence state molysite |
| CN112079393B (en) * | 2020-09-25 | 2022-06-14 | 常熟理工学院 | Method for preparing potassium ferrate by using low-temperature plasma technology |
| CN113582236A (en) * | 2021-08-30 | 2021-11-02 | 陕西省石油化工研究设计院 | Preparation method of potassium ferrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4606843A (en) * | 1985-01-24 | 1986-08-19 | Olin Corporation | Process for producing a dried, stable mixture of alkali metal or alkaline earth metal ferrate (VI) compounds with hydroxides and carbonates |
| CN1749166A (en) * | 2005-11-03 | 2006-03-22 | 深圳职业技术学院 | Process for preparing solid potassium ferrate |
| CN1752002A (en) * | 2005-10-28 | 2006-03-29 | 厦门大学 | Method for simultaneously preparing two ferrates |
| CN101597087A (en) * | 2008-06-05 | 2009-12-09 | 张亮 | A kind of drinking water treatment agent---the quick synthesis method of potassium ferrate |
-
2014
- 2014-09-23 CN CN201410491153.0A patent/CN104261481B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4606843A (en) * | 1985-01-24 | 1986-08-19 | Olin Corporation | Process for producing a dried, stable mixture of alkali metal or alkaline earth metal ferrate (VI) compounds with hydroxides and carbonates |
| CN1752002A (en) * | 2005-10-28 | 2006-03-29 | 厦门大学 | Method for simultaneously preparing two ferrates |
| CN1749166A (en) * | 2005-11-03 | 2006-03-22 | 深圳职业技术学院 | Process for preparing solid potassium ferrate |
| CN101597087A (en) * | 2008-06-05 | 2009-12-09 | 张亮 | A kind of drinking water treatment agent---the quick synthesis method of potassium ferrate |
Non-Patent Citations (1)
| Title |
|---|
| "高铁酸钾制备新方法与光谱表征";郑怀礼等;《光谱学与光谱分析》;20101031;第30卷(第10期);第2646-2649页 * |
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