CN104876278B - Method is prepared in the atomization of a kind of potassium ferrate - Google Patents
Method is prepared in the atomization of a kind of potassium ferrate Download PDFInfo
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- CN104876278B CN104876278B CN201510235102.6A CN201510235102A CN104876278B CN 104876278 B CN104876278 B CN 104876278B CN 201510235102 A CN201510235102 A CN 201510235102A CN 104876278 B CN104876278 B CN 104876278B
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- potassium ferrate
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- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000889 atomisation Methods 0.000 title claims abstract description 14
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 11
- 150000002505 iron Chemical class 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000460 chlorine Substances 0.000 claims abstract description 8
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 8
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- 239000012047 saturated solution Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 229910000358 iron sulfate Inorganic materials 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium superoxide Chemical compound [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 description 2
- 238000009279 wet oxidation reaction Methods 0.000 description 2
- GPZVUOSXHJGAKW-UHFFFAOYSA-N Cl[O-].[K+].[Na+].Cl[O-] Chemical compound Cl[O-].[K+].[Na+].Cl[O-] GPZVUOSXHJGAKW-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006199 nebulizer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- -1 purity is 99.2% Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
Abstract
The present invention relates to environmental conservation material for water treatment technical field; more specifically; method is prepared in the atomization relating to a kind of potassium ferrate; it is that iron salt solutions and saturated postassium hypochlorite solution are atomized respectively; and be passed through in high-pressure reactor together with chlorine; at the crystal that 5～35 DEG C of reactions obtain, through drip washing, obtain potassium ferrate after drying.The preparation of the method raw material is simple, reaction condition is gentle, compared with the preparation method of existing potassium ferrate, owing in preparation process, main reactant is in spray pattern, while improve reaction efficiency, also improves the purity of product；Preparation-obtained potassium ferrate purity reaches more than 99.0%.
Description
Technical field
The present invention relates to environmental conservation material for water treatment technical field, method is prepared in the atomization more particularly, to a kind of potassium ferrate.
Background technology
Potassium ferrate is paid close attention in water treatment field widely so that it has strong oxidizing property, in aqueous with high ferro acid group FeO4 2-Form exists, and has extremely strong oxidisability, and the oxidation-reduction potential under the conditions of acidity and alkalescence is respectively+2.20V and+0.72V.Potassium ferrate has collection and aoxidizes, adsorbs, flocculates and help the feature being condensated as a whole, and is mainly used in industrial wastewater and city domestic sewage processes, be also used for drinking water disinfection, can quickly kill the antibacterial in water and virus.Owing to potassium ferrate not only using effect is good, and will not produce in application process and be hazardous to the human body, be a kind of efficient and the New Type Water Treatment Chemicals of non-secondary pollution, in terms of water process, demonstrate good application prospect.
Ferrate preparation method mainly includes high-temperature melting method, electrolysis and wet oxidation method；As long as high-temperature melting method utilizes oxidant potassium peroxide, sodium peroxide, potassium peroxydisulfate or potassium nitrate; simultaneously with ferrum or ferrum oxide as source of iron; and generate potassium ferrate with the reaction of melt and dissolved state under the conditions of 500 DEG C of high temperature above; CNl769186A, US4385045, US4551326, US4545974, US20050253171 and US20100151049 patent have employed the method; but this process reaction is uneven; whole experimentation needs to be passed through nitrogen protection always, and mixture separates difficulty；Electrolysis is to use nickel plate and iron plate respectively as negative electrode and anode, using concentrated base as the electrolyte of reaction, is electrolysed.On the iron plate as reaction anode, Fe and Fe3+It is oxidized to FeO4 2-, finally containing FeO4 2-Anodic dissolution in add concentrated base KOH, i.e. have K2FeO4Crystal separates 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 big, on-the-spot operating cost is high, technique prepares productivity and product purity is all not sufficiently stable, and the by-product produced in experimentation is more；Wet oxidation method is addition sodium hypochlorite (potassium) solution in alkaline solution, after being sufficiently mixed, adds source of iron, just has Na2Fe04 to generate in the solution, be eventually adding potassium hydroxide solution, prepares potassium ferrate.nullPatent 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 persulfate (HSO5 -) Oxidation of Fe3+Prepare ferrate, but single persulfate source lacks.It is a kind of widely used method that wet method prepares potassium ferrate.Complicated technological process allows wet method prepare ferrate has strict requirements to process conditions；The preparation hypochlorite process that in experimentation, the conversion ratio of source of iron is the highest and traditional, there is also course of reaction more violent, and raw material utilizes the shortcomings such as insufficient.
Summary of the invention
The drawbacks described above being to overcome prior art to exist is solved the technical problem that, it is provided that method is prepared in the atomization of a kind of new potassium ferrate used by the present invention.
Second object of the present invention is to provide the potassium ferrate that said method prepares.
It is an object of the invention to be achieved by the following technical programs:
Method is prepared in the atomization of a kind of potassium ferrate, iron salt solutions and saturated postassium hypochlorite solution is atomized respectively, and is passed through together with chlorine in high-pressure reactor, at the crystal that 5～35 DEG C of reactions obtain, through drip washing, obtains potassium ferrate after drying；Described iron salt solutions is iron nitrate solution, ferric chloride solution and iron sulfate.
The preparation of potassium ferrate is typically in the basic conditions, by hypochlorite oxidation's ferric iron；On the premise of the present invention is in compliance with mentioned above principle simultaneously, a kind of method providing atomization to prepare potassium ferrate, be iron salt solutions and saturated postassium hypochlorite solution are atomized by nebulizer respectively after, be passed through chlorine and react, reaction condition is gentle, and reaction efficiency, product purity are greatly improved.
Applicant is found by research, and during potassium ferrate is prepared in atomization, postassium hypochlorite solution must be saturated, and now potassium ferrate productivity and purity are the highest.
Preferably, described saturated postassium hypochlorite solution is obtained by following steps: S1. adds calcium hypochlorite in potassium hydroxide solution, sucking filtration retain filtrate after reaction；S2. in filtrate, add the potassium hydroxide solution described in S1 of equivalent, obtain saturated postassium hypochlorite solution.
Preferably, also it is saturated solution when iron salt solutions.
Further, when being ferric nitrate when selecting iron salt solutions, purity and the productivity of the potassium ferrate prepared are the highest.
Preferably, the concentration of potassium hydroxide described in S1 is not less than 14M, and the amount of every liter of potassium hydroxide addition calcium hypochlorite is 500～700g.
Specifically, 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 sucking filtration is that the filter cloth using 800～1500 mesh is carried out；Described crystal respectively with normal hexane, absolute methanol drip washing, after be vacuum dried in the environment of 65～75 DEG C 3～5 hours and obtain potassium ferrate.
Compared with prior art, the method have the advantages that
Method is prepared in the atomization that the invention provides a kind of potassium ferrate, it is that the raw material preparing potassium ferrate is first atomized, after in the presence of chlorine reaction under high pressure obtain, the preparation of the method raw material is simple, reaction condition is gentle, compared with the preparation method of existing potassium ferrate, owing in preparation process, main reactant is in spray pattern, while improve reaction efficiency, also improve the purity of product；Preparation-obtained potassium ferrate purity reaches more than 99.0%.
Detailed description of the invention
Below by embodiment specific descriptions further to the present invention.If following used experimental technique is without specified otherwise, the method being the existing routine of the art, the dispensing used or material, if no special instructions, it is by the available dispensing of commercial sources or material；The present invention should not necessarily 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 calcium hypochlorite solid according to every liter；Fully use the filter cloth suction filtering of 800 mesh after reaction, retain filtrate；
S2. in filtrate, add the KOH solution of equal-volume 14mol/L, obtain saturated postassium hypochlorite solution;
Every liter of deionized water solution adds 150g nitric hydrate ferrum the most at normal temperatures, and uniform 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, are also simultaneously directed in high-pressure reactor by chlorine, and temperature of reactor keeps 20 DEG C, and 90min obtains potassium ferrate crystalline solid；
The most respectively with normal hexane and absolute methanol drip washing potassium ferrate crystal 5 times, and in the environment of 65 DEG C, be vacuum dried 3 hours, obtain end product potassium ferrate, purity is 99.2%, and product decomposition of 30d when room 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 calcium hypochlorite solid according to every liter；Fully use the filter cloth suction filtering of 1000 mesh after reaction, retain filtrate；
S2. in filtrate, add the KOH solution of equal-volume 15mol/L, obtain saturated postassium hypochlorite solution；
Every liter of deionized water solution adds 160g nitric hydrate ferrum the most at normal temperatures, and uniform by magnetic stirrer, obtain saturated iron nitrate solution；
S4. being atomized respectively by two kinds of saturated solution nonionic nebulizers, and import in high-pressure reactor, be also simultaneously directed in high-pressure reactor by chlorine, temperature of reactor keeps 25 DEG C, and 90min obtains potassium ferrate crystalline solid；
The most respectively with normal hexane and absolute methanol drip washing potassium ferrate crystal 4 times, and in the environment of 70 DEG C, being vacuum dried 3.5 hours, obtain end product potassium ferrate, purity is 99.4%.
Comparative example
1
Experimental technique is with embodiment 1, unlike Wei Yi, postassium hypochlorite solution used is not saturated solution, end product potassium ferrate is detected, result shows: response time 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 room temperature keeps in Dark Place is more than 5%.
Comparative example
2
Experimental technique with embodiment 1, unique unlike, replace ferric nitrate with iron chloride, end product potassium ferrate detected, result shows: response time 90min, and purity is 97.7%.
Experimental technique with embodiment 1, unique unlike, replace ferric nitrate with iron sulfate, end product potassium ferrate detected, result shows: response time 90min, and purity is 92.4%.
Comparative example
3
Experimental technique with embodiment 1, unique unlike, iron nitrate solution used is not saturated solution, detects end product potassium ferrate, and result shows: response time 90min, and purity is 83.6%.
Comparative example
4
Experimental technique with embodiment 1, unique unlike, postassium hypochlorite solution used and iron nitrate solution are not saturated solution, detect end product potassium ferrate, and result show: response time 90min, are little to generation potassium ferrate.
Comparative example
5
Experimental technique with embodiment 1, unique unlike, high-pressure reactor is not passed through chlorine, end product potassium ferrate is detected, result shows: response time 90min, and purity is 89.1%.
Comparative example
6
Experimental technique with embodiment 1, unique unlike, high-pressure reactor is passed through O3, end product potassium ferrate is detected, result shows: response time 90min, purity 85.7%.
Claims (5)
1. method is prepared in the atomization of a potassium ferrate, it is characterised in that iron salt solutions and saturated postassium hypochlorite solution is atomized respectively, and is passed through together with chlorine in high-pressure reactor, at the crystal that 5～35 DEG C of reactions obtain, through drip washing, obtains potassium ferrate after drying；Described iron salt solutions is iron nitrate solution, ferric chloride solution and ferrum sulfuricum oxydatum solutum；Described saturated postassium hypochlorite solution is obtained by following steps: S1. adds calcium hypochlorite in potassium hydroxide solution, sucking filtration retain filtrate after reaction；S2. in filtrate, add the potassium hydroxide solution described in S1 of equivalent, obtain saturated postassium hypochlorite solution.
Atomization preparation method the most according to claim 1, it is characterised in that described iron salt solutions is saturated iron salt solutions.
Atomization preparation method the most according to claim 1, it is characterised in that the concentration of potassium hydroxide described in S1 is not less than 14M, and the amount of every liter of potassium hydroxide addition calcium hypochlorite is 500～700g.
4. prepare method according to the atomization described in any one of claims 1 to 3, it is characterised in that described crystal respectively with normal hexane, absolute methanol drip washing, after be vacuum dried in the environment of 65～75 DEG C 3～5 hours and obtain potassium ferrate.
5. prepare method according to the atomization described in any one of claims 1 to 3, it is characterised in that described sucking filtration is that the filter cloth using 800～1500 mesh is carried out.
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| 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 |
| 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 |
Citations (4)
| 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 |
-
2015
- 2015-05-11 CN CN201510235102.6A patent/CN104876278B/en not_active Expired - Fee Related
Patent Citations (4)
| 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 |
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