CN104876278A - Atomization preparation method of potassium ferrate - Google Patents

Atomization preparation method of potassium ferrate Download PDF

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CN104876278A
CN104876278A CN201510235102.6A CN201510235102A CN104876278A CN 104876278 A CN104876278 A CN 104876278A CN 201510235102 A CN201510235102 A CN 201510235102A CN 104876278 A CN104876278 A CN 104876278A
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potassium
potassium ferrate
solution
preparation
ferrate
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CN201510235102.6A
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CN104876278B (en
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曹刚
黄郑郑
罗恺
李紫惠
邵基伦
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Jinan University
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Jinan University
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Abstract

The invention relates to the technical field of environment-friendly water treatment materials, particularly an atomization preparation method of potassium ferrate, which comprises the following steps: respectively atomizing an iron salt solution and a saturated potassium hypochlorite solution, introducing the atomized iron salt solution and saturated potassium hypochlorite solution into a high-pressure reactor together with chlorine, reacting at 5-35 DEG C to obtain a crystal, eluting and drying to obtain the potassium ferrate. The method has the advantages of simple raw material preparation and mild reaction conditions. Compared with the existing potassium ferrate preparation method, the method provided by the invention enhances the reaction efficiency and the product purity since the main reactants are in the atomization state in the preparation process. The purity of the obtained potassium ferrate is up to 99.0% above.

Description

A kind of atomization preparation method of potassium ferrate
Technical field
The present invention relates to environment protection material for water treatment technical field, more specifically, relate to a kind of atomization preparation method of potassium ferrate.
Background technology
Potassium ferrate has strong oxidizing property with it and is paid close attention to widely in water treatment field, in aqueous with high ferro acid group FeO 4 2-form exists, and has extremely strong oxidisability, and the redox potential under acidity and alkaline condition is respectively+2.20V and+0.72V.Potassium ferrate has collection and is oxidized, adsorbs, flocculates and helps the feature be condensated as a whole, and is mainly used in trade effluent and city domestic sewage process, also for drinking water disinfection, can kills the bacterium in water and virus fast.Due to potassium ferrate, not only result of use is good, and can not produce in application process and have harm to human body, is a kind of efficient and New Type Water Treatment Chemicals of non-secondary pollution, demonstrates good application prospect in water treatment.
Ferrate preparation method mainly comprises high-temperature melting method, electrolytic process and wet oxidation method; As long as high-temperature melting method utilizes oxygenant Potassium peroxide, sodium peroxide, Potassium Persulphate or saltpetre, simultaneously with iron or ferric oxide for source of iron, and potassium ferrate is generated with melt and dissolved state reaction under hot conditions more than 500 DEG C, CNl769186A, US4385045, US4551326, US4545974, US20050253171 and US20100151049 patent have employed the method, but this process reaction is uneven, whole experimentation needs to pass into nitrogen protection always, and mixture separation is difficult; Electrolytic process uses nickel plate and iron plate respectively as negative electrode and anode, using the electrolytic solution of concentrated base as reaction, carries out electrolysis.On the iron plate as reaction anode, Fe and Fe 3+be oxidized to FeO 4 2-, finally containing FeO 4 2-anodic dissolution in add concentrated base KOH, namely have K 2feO 4crystal is separated out, the patent such as patent US4451338, US4435257, US4435256, US7045051, US20030159942, CN1488782A, CNl740398A, CN1900365ACN101187028A, CN101525754A, CN101713078A, 102560522A and CN103663563A have employed the method, but this method energy consumption is large, on-the-spot running cost is high, technique prepares productive rate and product purity is stable all not, and the by product produced in experimentation is more; Wet oxidation method is in basic solution, add clorox (potassium) solution, fully after mixing, then adds source of iron, just has Na2Fe04 to generate in the solution, finally add potassium hydroxide solution, obtained potassium ferrate.Patent CN1329182A, CN1613778A, CNl749166A, CN1301912C, CN101117240A, CN101318707A, CN101503216A, CN101597087A, CN101955230B, CN102161513B, CN102701286A, CN103193275A, CN103265084A, CN103145189A, US20020121482, US20020155044, US20030146169, US20090120802, US20110036725Al, the patents such as US20120175314Al have employed the method.Patent US5746994 have employed single persulphate (HSO 5 -) Oxidation of Fe 3+prepare ferrate, but single persulphate source lacks.Wet-layer preparation potassium ferrate is a kind of widely used method.Complicated technical process allows wet-layer preparation ferrate have strict requirement to processing condition; , also there is reaction process comparatively violent, the shortcomings such as prepared using is insufficient in the preparation hypochlorite process that in experimentation, the transformation efficiency of source of iron is high and not traditional yet.
Summary of the invention
The technical problem of the present invention's solution used is the above-mentioned defect overcoming prior art existence, provides a kind of atomization preparation method of new potassium ferrate.
Second object of the present invention is to provide the potassium ferrate that aforesaid method prepares.
The object of the invention is to be achieved by the following technical programs:
An atomization preparation method for potassium ferrate, is atomized iron salt solutions and saturated potassium hypochlorite solution respectively, and passes into together with chlorine in high-pressure reactor, at the crystal that 5 ~ 35 DEG C are obtained by reacting, after drip washing, drying, obtain potassium ferrate; Described iron salt solutions is iron nitrate solution, ferric chloride Solution and ferric sulfate.
The preparation of potassium ferrate normally in the basic conditions, by hypochlorite oxidation's ferric iron; The present invention is under the prerequisite following mentioned above principle simultaneously, thering is provided a kind of atomization to prepare the method for potassium ferrate, is, after iron salt solutions and saturated potassium hypochlorite solution being atomized respectively by spraying gun, passing into chlorine and react, reaction conditions is gentle, and reaction efficiency, product purity improve greatly.
Applicant is found by research, and prepare in the process of potassium ferrate in atomization, potassium hypochlorite solution must be saturated, and now potassium ferrate productive rate and purity are all higher.
Preferably, described saturated potassium hypochlorite solution is obtained by following steps: S1. adds Losantin in potassium hydroxide solution, and suction filtration after reaction also retains filtrate; S2. in filtrate, add the potassium hydroxide solution described in S1 of equivalent, obtain saturated potassium hypochlorite solution.
Preferably, when iron salt solutions is also saturated solution.
Further, when being iron nitrate when selecting iron salt solutions, the purity of the potassium ferrate prepared and productive rate are all higher.
Preferably, described in S1, the concentration of potassium hydroxide is not less than 14M, and the amount that often liter of potassium hydroxide adds Losantin is 500 ~ 700g.
Particularly, the concentration of potassium hydroxide described in S1 is 12 ~ 16M.
In the preparation method of the above-mentioned potassium ferrate of the present invention, described suction filtration is that use 800 ~ 1500 object filter cloth carries out; Described crystal uses normal hexane, anhydrous methanol drip washing respectively, after under the environment of 65 ~ 75 DEG C vacuum-drying 3 ~ 5 hours obtain potassium ferrate.
Compared with prior art, the present invention has following beneficial effect:
The invention provides a kind of atomization preparation method of potassium ferrate, that the raw material preparing potassium ferrate is first atomized, after under the existence of chlorine reaction under high pressure obtain, the preparation of the method raw material is simple, reaction conditions is gentle, compared with the preparation method of existing potassium ferrate, because in preparation process, main reactant is in atomizing state, while improve reaction efficiency, also improve the purity of product; Preparation-obtained potassium ferrate purity reaches more than 99.0%.
Embodiment
Below by embodiment, the present invention is specifically described further.If following used experimental technique is without specified otherwise, be the method for the existing routine of the art, the batching used or material, if no special instructions, be by the available batching of commercial sources or material; The present invention should not be limited to scope of embodiments.
embodiment 1
The preparation of the present embodiment potassium ferrate comprises the following steps:
S1. compound concentration is the KOH solution of 14mol/L, adds 550g Losantin solid according to often liter; Use 800 object filter cloth suction filterings after abundant reaction, retain filtrate;
S2. in filtrate, add the KOH solution of equal-volume 14mol/L, obtain saturated potassium hypochlorite solution;
S3. 150g nitric hydrate iron is added in often liter of deionized water solution at normal temperatures, and even by magnetic stirrer, obtain saturated iron nitrate solution;
S4. the two kinds of saturated solution jet flow type atomizers obtained by S2 and S3 are atomized respectively, and import in high-pressure reactor, and also imported in high-pressure reactor by chlorine, temperature of reactor keeps 20 DEG C, 90min, obtains potassium ferrate xln simultaneously;
S5. use normal hexane and anhydrous methanol drip washing potassium ferrate crystal 5 times respectively, and under the environment of 65 DEG C, vacuum-drying 3 hours, obtains final product potassium ferrate, purity is 99.2%, and product decomposition of 30d when normal temperature keeps in Dark Place is less than 0.3%.
embodiment 2
The preparation of the present embodiment potassium ferrate comprises the following steps:
S1. compound concentration is the KOH solution of 15mol/L, adds 600g Losantin solid according to often liter; Use 1000 object filter cloth suction filterings after abundant reaction, retain filtrate;
S2. in filtrate, add the KOH solution of equal-volume 15mol/L, obtain saturated potassium hypochlorite solution;
S3. 160g nitric hydrate iron is added in often liter of deionized water solution at normal temperatures, and even by magnetic stirrer, obtain saturated iron nitrate solution;
S4. be atomized respectively by two kinds of saturated solution nonionic spraying guns, and import in high-pressure reactor, also imported in high-pressure reactor by chlorine, temperature of reactor keeps 25 DEG C, 90min, obtains potassium ferrate xln simultaneously;
S5. use normal hexane and anhydrous methanol drip washing potassium ferrate crystal 4 times respectively, and under the environment of 70 DEG C, vacuum-drying 3.5 hours, obtains final product potassium ferrate, purity is 99.4%.
comparative example 1
Experimental technique is with embodiment 1, uniquely unlike, potassium hypochlorite solution used is not saturated solution, final product potassium ferrate is detected, result shows: reaction times 90min, and the potassium ferrate of generation is little, in few potassium ferrate, potassium ferrate purity is only 78%, and product decomposition of 30d when normal temperature keeps in Dark Place is greater than 5%.
comparative example 2
Experimental technique with embodiment 1, uniquely unlike, replace iron nitrate with iron(ic) chloride, final product potassium ferrate detected, result show: reaction times 90min, purity is 97.7%.
Experimental technique with embodiment 1, uniquely unlike, replace iron nitrate with ferric sulfate, final product potassium ferrate detected, result show: reaction times 90min, purity is 92.4%.
comparative example 3
Experimental technique with embodiment 1, uniquely unlike, iron nitrate solution used is not saturated solution, detects final product potassium ferrate, result show: reaction times 90min, purity is 83.6%.
comparative example 4
Experimental technique with embodiment 1, uniquely unlike, potassium hypochlorite solution used and iron nitrate solution are not all saturated solution, detect final product potassium ferrate, result show: reaction times 90min, almost can not generate potassium ferrate.
comparative example 5
Experimental technique with embodiment 1, uniquely unlike, do not pass into chlorine in high-pressure reactor, final product potassium ferrate detected, result show: reaction times 90min, purity is 89.1%.
comparative example 6
Experimental technique with embodiment 1, uniquely unlike, pass into O in high-pressure reactor 3, detect final product potassium ferrate, result shows: reaction times 90min, purity 85.7%.

Claims (6)

1. an atomization preparation method for potassium ferrate, is characterized in that, iron salt solutions and saturated potassium hypochlorite solution is atomized respectively, and passes into together with chlorine in high-pressure reactor, at the crystal that 5 ~ 35 DEG C are obtained by reacting, after drip washing, drying, obtain potassium ferrate; Described iron salt solutions is iron nitrate solution, ferric chloride Solution and ferrum sulfuricum oxydatum solutum.
2. atomization preparation method according to claim 1, is characterized in that, described iron salt solutions is saturated iron salt solutions.
3. atomization preparation method according to claim 1, is characterized in that, described saturated potassium hypochlorite solution is obtained by following steps: S1. adds Losantin in potassium hydroxide solution, and suction filtration after reaction also retains filtrate; S2. in filtrate, add the potassium hydroxide solution described in S1 of equivalent, obtain saturated potassium hypochlorite solution.
4. atomization preparation method according to claim 3, is characterized in that, described in S1, the concentration of potassium hydroxide is not less than 14M, and the amount that often liter of potassium hydroxide adds Losantin is 500 ~ 700g.
5. the atomization preparation method according to any one of Claims 1-4, is characterized in that, described crystal uses normal hexane, anhydrous methanol drip washing respectively, after under the environment of 65 ~ 75 DEG C vacuum-drying 3 ~ 5 hours obtain potassium ferrate.
6. the atomization preparation method according to any one of Claims 1-4, is characterized in that, described suction filtration is that use 800 ~ 1500 object filter cloth carries out.
CN201510235102.6A 2015-05-11 2015-05-11 Method is prepared in the atomization of a kind of potassium ferrate Expired - Fee Related CN104876278B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112079393A (en) * 2020-09-25 2020-12-15 常熟理工学院 Method for preparing potassium ferrate by using low-temperature plasma technology

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4451338A (en) * 1981-03-23 1984-05-29 Olin Corporation Process for making a calcium/sodium ferrate adduct by the electrochemical formation of sodium ferrate
CN101117240A (en) * 2007-07-07 2008-02-06 黄山学院 Preparation method of 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
CN103663563A (en) * 2012-09-22 2014-03-26 金华弗兰德环保科技有限公司 Preparation method of potassium ferrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4451338A (en) * 1981-03-23 1984-05-29 Olin Corporation Process for making a calcium/sodium ferrate adduct by the electrochemical formation of sodium ferrate
CN101117240A (en) * 2007-07-07 2008-02-06 黄山学院 Preparation method of 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
CN103663563A (en) * 2012-09-22 2014-03-26 金华弗兰德环保科技有限公司 Preparation method of potassium ferrate

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112079393A (en) * 2020-09-25 2020-12-15 常熟理工学院 Method for preparing potassium ferrate by using low-temperature plasma technology
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

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