CN105329949B - Method for in-situ preparation of ferrate by means of singlet oxygen - Google Patents
Method for in-situ preparation of ferrate by means of singlet oxygen Download PDFInfo
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- CN105329949B CN105329949B CN201510785791.8A CN201510785791A CN105329949B CN 105329949 B CN105329949 B CN 105329949B CN 201510785791 A CN201510785791 A CN 201510785791A CN 105329949 B CN105329949 B CN 105329949B
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- ferrate
- singlet oxygen
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
Abstract
The invention discloses a method for in-situ preparation of ferrate by means of singlet oxygen and relates to compound preparation methods. The method comprises the steps of mixing strong base with the catalyst pyruvic acid, adding the oxidizing agent peroxide (peroxymonosulfate or percarbonate), conducting even stirring, adding ferric salt quickly, and conducting stirring to obtain an atropurpureus ferrate solution. The peroxide is catalyzed by pyruvic acid to generate a dual-epoxy midbody, the dual-epoxy midbody reacts with the peroxide to generate singlet oxygen and pyruvic acid, the generated pyruvic acid is still used for catalyzing the peroxide and plays a role of cyclic catalysis in reaction, ferric salt is oxidized into ferrate by means of the generated high-activity singlet oxygen, and pyruvic acid also has a complexing action, so that the stability of the ferrate solution is improved and preparation is achieved. The catalyst pyruvic acid and the oxidizing agent peroxide are environmentally friendly, safe and free of side effect, preparation is easy and safe, the yield of the ferrate solution is high, the stability of the ferrate solution is high, and the ferrate solution is suitable for being prepared when needed.
Description
Technical field
The present invention relates to the preparation method of a compound is and in particular to one kind prepares ferric acid using singlet oxygen original position
The method of salt.
Background technology
Ferrate, as Green Oxidant, has oxidation, absorption, coprecipitated, sterilization, sterilized, except Multifunctional water purifications such as algaes
Characteristic, is a kind of preferable water treatment agent.But because the preparation condition of ferrate is quite harsh, sintetics purity is high,
Low yield, impurity are many, and ferrate easily decomposes it is difficult to preserve in water or under wet condition, therefore limits it and carries out greatly
The application of scale.
At present, the method preparing ferrate mainly has three kinds: (l) wet oxidation process, i.e. hypochlorite oxidation method, research
The comparison carried out is early, and comparison of technology is ripe, and the yield of sintetics and purity are high, but operating procedure excessively various it is desirable to
Control temperature alkali consumption in zero degrees celsius, preparation big, seriously polluted；(2) electrochemical process, also known as electrolysis, simple to operate,
Raw materials consumption is few, but power consumption is big, and accessory substance is many, and influence factor is many, low yield；(3) dry method, is also called fusion method and height
Warm peroxidating method, the purity of sintetics and yield are higher, but operation needs higher temperature, there is the danger of blast.
Patent us005746994a prepares ferrate using single persulfate oxidation ferric sulfate under strongly alkaline conditions, but
This method needs ice bath, and reaction temperature will control below 0 DEG C.Patent ep19820305914 utilize alkaline postassium hypochlorite and
Molysite prepares ferrate, but the ferrate solution due to producing is very unstable, and this patent adopts dimethyl sulfoxide, dimethyl
Sulfone, methyl alcohol etc. purifies ferrate.By the use of beta oxidation iron as source of iron in patent us5217584, using the sodium comprising iodine or tellurium
Salt or sylvite, as stabilizer, prepare ferrate, 18～25 DEG C of reaction temperature, reaction time 1～6h using hypochlorous acid oxidization.
Molysite, activator, alkali are maintained agent to mix by patent cn103723772a, are heated to temperature and are 30 DEG C～398 DEG C, then by oxygen
Agent solution wherein, prepared composite ferrate chemicals.Patent cn101497461a describes one kind under the conditions of microwave
With ferroso-ferric oxide for the method for source of iron rapid preparing ferrate solution.
The method preparing ferrate solution using singlet oxygen original position is had not seen in above-mentioned patent.
Singlet oxygen (1o2) it is a kind of molecular oxygen being in excitation state, with superoxide radicalHydroxyl radical free radical (
Oh), potentiometric titrationsIsoreactivity oxygen species are similar to, and chemical property is active, unstable, extensively deposits in nature
It is being one of the longest active oxygen being related in the fields such as chemistry, environment, medical science, having that oxidability is strong, reactivity is high, a survival
Time is short, the features such as do not produce poisonous and harmful accessory substance after oxidation, belong to green, environmentally friendly oxidant.
Content of the invention
It is an object of the invention to provide a kind of method preparing ferrate using singlet oxygen original position, solve existing high ferro
Hydrochlorate preparation method operating process is complicated, the problem of products therefrom stability difference.
The present invention a kind of using singlet oxygen original position prepare ferrate method through the following steps that realize:
First, highly basic and catalyst are in molar ratio 1:(0.1～10) it is added in reactor after mixing, add oxidant, stirring
Uniformly, obtain solution；2nd, add molysite in the solution of step one, after stirring, that is, complete described utilization singlet oxygen former
The method that ferrate is prepared in position；
Wherein, pyruvic acid and the mol ratio of oxidant are 1:(1～10)；The mol ratio of oxidant and molysite be 1:(1～
10)；Described oxidant is peroxide；Described catalyst is pyruvic acid.
The present invention a kind of using singlet oxygen original position prepare ferrate Method And Principle as follows: first, acetone acid catalysis
Peroxide (peroxy-monosulfate or percarbonate) produces bis-epoxy intermediate；Then, bis-epoxy intermediate further with peroxide
Compound reaction generation singlet oxygen (1o2) and pyruvic acid, simultaneously bis-epoxy intermediate selfdecomposition also can be occurred to produce singlet oxygen
(1o2) and pyruvic acid, the pyruvic acid of generation continues to be catalyzed peroxide, plays the effect of circulation catalysis in the reaction；Produce is strong
Iron salt oxidization is ferrate by oxidisability singlet oxygen, reaches the purpose preparing ferrate in situ.Concrete reaction mechanism is shown in
Accompanying drawing 1.
A kind of method preparing ferrate using singlet oxygen original position of the present invention, has the advantage that
(1) environmentally friendly oxidant singlet oxygen (1o2) reactivity is strong, oxidation efficiency is high, oxidation after do not produce poisonous
Harmful side product.
(2) pyruvic acid, as one of the intermediate product of organism analytic metabolism, is the glucolytic final product of glucose, quilt
It is widely used in the processes such as food processing, therefore, pyruvic acid is as catalyst, safe and reliable, has no toxic side effect.
(3) pyruvic acid can increase the stability of ferrate solution with the ferrate complexing of original position preparation.
(4), as pulverulent solids, chemical property is steady for Green Oxidant peroxide (peroxy-monosulfate, percarbonate)
Fixed, shipping storage is convenient, moderate, is commercially easy to get, operation is simple, does not produce poisonous and harmful accessory substance after reaction.
(5) the method original position prepare that ferrate solution is simple to operate, safety it is not necessary to ice bath and heating, at room temperature
Can complete, be very suitable for existing existing system.
Brief description
Fig. 1 is a kind of method reaction mechanism figure preparing ferrate using singlet oxygen original position.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also includes between each specific embodiment
Any combination.
Specific embodiment one: present embodiment is a kind of method preparing ferrate using singlet oxygen original position is logical
Cross following steps realization: one, by highly basic and catalyst be 1:(0.1～10 in molar ratio) it is added in reactor after mixing,
Add oxidant, stir, obtain solution；2nd, add molysite in the solution of step one, stir, treat that solution is complete
Become atropurpureus, that is, complete the method that described utilization singlet oxygen original position prepares ferrate；
Wherein, pyruvic acid and the mol ratio of oxidant are 1:(1～10)；The mol ratio of oxidant and molysite be 1:(1～
10)；Described oxidant is peroxide；Described catalyst is pyruvic acid.
Present embodiment a kind of using singlet oxygen original position prepare ferrate Method And Principle as follows: first, pyruvic acid
Catalysis peroxide (peroxy-monosulfate or percarbonate) produces bis-epoxy intermediate；Then, bis-epoxy intermediate further with
Peroxide reactions generation singlet oxygen (1o2) and pyruvic acid, simultaneously bis-epoxy intermediate selfdecomposition also can be occurred to produce singlet
Oxygen (1o2) and pyruvic acid, the pyruvic acid of generation continues to be catalyzed peroxide, plays the effect of circulation catalysis in the reaction；Produce
Iron salt oxidization is ferrate by strong oxidizing property singlet oxygen, reaches the purpose preparing ferrate in situ, deposits simultaneously in solution
Pyruvic acid can play the effect of complexing so that ferrate solution can be with stable existence again.Concrete reaction mechanism is shown in accompanying drawing
1.
A kind of advantage of method preparing ferrate using singlet oxygen original position of present embodiment: (1) environmental friendliness
Type oxidant singlet oxygen (1o2) reactivity is strong, oxidation efficiency is high, oxidation after do not produce poisonous and harmful accessory substance.(2) acetone
One of sour intermediate product as organism analytic metabolism, is the glucolytic final product of glucose, is widely used in food and adds
The processes such as work, therefore, pyruvic acid is as catalyst, safe and reliable, has no toxic side effect.(3) pyruvic acid can be with original position preparation
Ferrate is complexed, and increases the stability of ferrate solution.(4) Green Oxidant peroxide (peroxy-monosulfate, percarbonic acid
Salt) as pulverulent solids, stable chemical nature, shipping storage is convenient, moderate, commercially it is easy to get, operation is simple, instead
Poisonous and harmful accessory substance is not produced after answering.(5) the method original position prepares that ferrate solution is simple to operate, safety is it is not necessary to ice
Bath and heating, can complete at room temperature, be very suitable for existing existing system.
Specific embodiment two: present embodiment from unlike specific embodiment one: described peroxide was one
The mixture that in sulfate, percarbonate, one or more are mixed by any ratio.Other identical with specific embodiment one.
Specific embodiment three: present embodiment from unlike specific embodiment one: peroxy-monosulfate was a sulphur
Sour sodium (nahso5), permonosulphuric acid potassium (khso5), permonosulphuric acid ammonium (nh4hso5), permonosulphuric acid calcium (ca (hso5)2), cross a sulphur
Sour magnesium (mg (hso5)2) one or more of the mixture that is mixed by any ratio.Other identical with specific embodiment one.
Specific embodiment four: present embodiment from unlike specific embodiment one: described molysite be iron chloride, chlorine
Change one or more of ferrous iron, ferric nitrate, ferrous nitrate, ferric sulfate, the ferrous sulfate mixture by any ratio.Other and tool
Body embodiment one is identical.
Specific embodiment five: present embodiment from unlike specific embodiment one: in step 2 add molysite, stir
Mix and become atropurpureus completely to solution, that is, complete the method that described utilization singlet oxygen original position prepares ferrate.Other with
Specific embodiment one is identical.
Specific embodiment six: present embodiment from unlike specific embodiment one: highly basic and catalyst molar ratio
For 1:(0.5～10).Other identical with specific embodiment one.
Specific embodiment seven: present embodiment from unlike specific embodiment one: highly basic and catalyst molar ratio
For 1:(1～10).Other identical with specific embodiment one.
Specific embodiment eight: present embodiment from unlike specific embodiment one: highly basic and catalyst molar ratio
For 1:(1～9).Other identical with specific embodiment one.
Specific embodiment nine: present embodiment from unlike specific embodiment one: highly basic and catalyst molar ratio
For 1:(1～8).Other identical with specific embodiment one.
Specific embodiment ten: present embodiment from unlike specific embodiment one: highly basic and catalyst molar ratio
For 1:(1～7).Other identical with specific embodiment one.
Specific embodiment 11: present embodiment from unlike specific embodiment one: highly basic and catalyst mole
Than for 1:(1～6).Other identical with specific embodiment one.
Specific embodiment 12: present embodiment from unlike specific embodiment one: highly basic and catalyst mole
Than for 1:(1～5).Other identical with specific embodiment one.
Specific embodiment 13: present embodiment from unlike specific embodiment one: highly basic and catalyst mole
Than for 1:(1～4).Other identical with specific embodiment one.
Specific embodiment 14: present embodiment from unlike specific embodiment one: highly basic and catalyst mole
Than for 1:(1～3).Other identical with specific embodiment one.
Specific embodiment 15: present embodiment from unlike specific embodiment one: highly basic and catalyst mole
Than for 1:(1～2).Other identical with specific embodiment one.
Specific embodiment 16: present embodiment from unlike specific embodiment one: pyruvic acid and oxidant
Mol ratio is 1:(1～9).Other identical with specific embodiment one.
Specific embodiment 17: present embodiment from unlike specific embodiment one: pyruvic acid and oxidant
Mol ratio is 1:(2～9).Other identical with specific embodiment one.
Specific embodiment 18: present embodiment from unlike specific embodiment one: pyruvic acid and oxidant
Mol ratio is 1:(3～8).Other identical with specific embodiment one.
Specific embodiment 19: present embodiment from unlike specific embodiment one: pyruvic acid and oxidant
Mol ratio is 1:(4～7).Other identical with specific embodiment one.
Specific embodiment 20: present embodiment from unlike specific embodiment one: pyruvic acid and oxidant
Mol ratio is 1:(4～6).Other identical with specific embodiment one.
Specific embodiment 21: present embodiment from unlike specific embodiment one: pyruvic acid and oxidant
Mol ratio be 1:5.Other identical with specific embodiment one.
Specific embodiment 22: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(1～9).Other identical with specific embodiment one.
Specific embodiment 23: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(1～8).Other identical with specific embodiment one.
Specific embodiment 24: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(1～7).Other identical with specific embodiment one.
Specific embodiment 25: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(1～6).Other identical with specific embodiment one.
Specific embodiment 26: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(1～5).Other identical with specific embodiment one.
Specific embodiment 27: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(1～4).Other identical with specific embodiment one.
Specific embodiment 28: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:(2～4).Other identical with specific embodiment one.
Specific embodiment 29: present embodiment from unlike specific embodiment one: oxidant and molysite
Mol ratio is 1:3.Other identical with specific embodiment one.
By following examples checking beneficial effects of the present invention:
Embodiment 1
The present embodiment a kind of using singlet oxygen original position prepare ferrate method through the following steps that realize:
A, NaOH and catalyst pyruvic acid are added in reactor, the mol ratio wherein controlling NaOH and pyruvic acid is 1:2；
B, in step a resulting solution, add oxidant permonosulphuric acid sodium, stir, wherein control pyruvic acid and permonosulphuric acid sodium
Mol ratio is 1:5；C, add ferric nitrate in step b resulting solution, stirring, wherein control rubbing of permonosulphuric acid sodium and ferric nitrate
That ratio is 1:3, treats that solution becomes atropurpureus completely, that is, completes to prepare ferrate solution using singlet oxygen original position.This enforcement
The ferrate solution of example preparation can preserve 8～15 days in refrigerator cold-storage.
Embodiment 2
The present embodiment a kind of using singlet oxygen original position prepare ferrate method through the following steps that realize:
A, potassium hydroxide and catalyst pyruvic acid are added in reactor, the mol ratio wherein controlling potassium hydroxide and pyruvic acid is 1:2；
B, add oxidation agent sodium percarbonate in step a resulting solution, stir, wherein control pyruvic acid and SODIUM PERCARBONATE mole
Than for 1:3；C, add iron chloride, stirring in step b resulting solution, the mol ratio wherein controlling SODIUM PERCARBONATE and iron chloride is
1:5, treats that solution becomes atropurpureus completely, that is, complete to prepare ferrate solution using singlet oxygen original position.Prepared by the present embodiment
Ferrate solution can preserve in refrigerator cold-storage 10～20 days.
Embodiment 3
The present embodiment a kind of using singlet oxygen original position prepare ferrate method through the following steps that realize:
A, potassium hydroxide and catalyst pyruvic acid are added in reactor, the mol ratio wherein controlling potassium hydroxide and pyruvic acid is 1:3；
B, add oxidation agent sodium percarbonate in step a resulting solution, stir, wherein control pyruvic acid and SODIUM PERCARBONATE mole
Than for 1:5；C, add iron chloride, stirring in step b resulting solution, the mol ratio wherein controlling SODIUM PERCARBONATE and iron chloride is
1:5, treats that solution becomes atropurpureus completely, that is, complete to prepare ferrate solution using singlet oxygen original position.
Embodiment 4
The present embodiment a kind of using singlet oxygen original position prepare ferrate method through the following steps that realize:
A, potassium hydroxide and catalyst pyruvic acid are added in reactor, the mol ratio wherein controlling potassium hydroxide and pyruvic acid is 1:4；
B, add oxidation agent sodium percarbonate in step a resulting solution, stir, wherein control pyruvic acid and SODIUM PERCARBONATE mole
Than for 1:5；C, add iron chloride, stirring in step b resulting solution, the mol ratio wherein controlling SODIUM PERCARBONATE and iron chloride is
1:3, treats that solution becomes atropurpureus completely, that is, complete to prepare ferrate solution using singlet oxygen original position.
Embodiment 5
The present embodiment a kind of using singlet oxygen original position prepare ferrate method through the following steps that realize:
A, potassium hydroxide and catalyst pyruvic acid are added in reactor, the mol ratio wherein controlling potassium hydroxide and pyruvic acid is 1:5；
B, add oxidation agent sodium percarbonate in step a resulting solution, stir, wherein control pyruvic acid and SODIUM PERCARBONATE mole
Than for 1:3；C, add iron chloride, stirring in step b resulting solution, the mol ratio wherein controlling SODIUM PERCARBONATE and iron chloride is
1:3, treats that solution becomes atropurpureus completely, that is, complete to prepare ferrate solution using singlet oxygen original position.
Claims (7)
1. a kind of using singlet oxygen original position prepare ferrate method it is characterised in that it through the following steps that realize
:
First, highly basic and catalyst are in molar ratio 1:(0.1～10) it is added in reactor after mixing, add oxidant,
Stir, obtain solution；2nd, add molysite in the solution of step one, after stirring, that is, complete described utilization singlet
The method that oxygen original position prepares ferrate；
Wherein, pyruvic acid and the mol ratio of oxidant are 1:(1～10)；Oxidant is 1:(1～10 with the mol ratio of molysite)；Institute
The oxidant stated is peroxide；Described catalyst is pyruvic acid；Described peroxide is peroxy-monosulfate, in percarbonate
One or more mixtures being mixed by any ratio；Peroxy-monosulfate be permonosulphuric acid sodium, permonosulphuric acid potassium, permonosulphuric acid ammonium,
The mixture that one or more of permonosulphuric acid calcium, permonosulphuric acid magnesium are mixed by any ratio；Percarbonate is SODIUM PERCARBONATE, mistake
One of potassium carbonate or two kinds of mixtures being mixed by any ratio.
2. according to claim 1 a kind of prepare the method for ferrate it is characterised in that institute using singlet oxygen original position
The highly basic stated be one or more of NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, potassium carbonate and saleratus by
Arbitrarily than mixture.
3. according to claim 1 a kind of prepare the method for ferrate it is characterised in that institute using singlet oxygen original position
State molysite be one or more of iron chloride, frerrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate by arbitrarily than
Mixture.
4. according to claim 1 a kind of using singlet oxygen original position prepare ferrate method it is characterised in that step
Add molysite in rapid two, stir and become atropurpureus completely to solution, that is, complete described utilization singlet oxygen and prepare high ferro in situ
The method of hydrochlorate.
5. according to claim 1 a kind of prepare the method for ferrate using singlet oxygen original position it is characterised in that strong
Alkali and catalyst molar ratio are 1:(0.5～10).
6. according to claim 1 a kind of prepare the method for ferrate it is characterised in that third using singlet oxygen original position
Ketone acid is 1:(1～5 with the mol ratio of oxidant).
7. according to claim 1 a kind of prepare the method for ferrate it is characterised in that oxygen using singlet oxygen original position
Agent is 1:(1～5 with the mol ratio of molysite).
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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 |
| CN101088926A (en) * | 2006-06-12 | 2007-12-19 | 深圳职业技术学院 | Combined water-treating farrate-fenton reagent process |
| CN103553203A (en) * | 2013-11-20 | 2014-02-05 | 哈尔滨理工大学 | Method for treating reverse osmosis concentrated solution by using singlet oxygen produced from peroxymonosulfate under induction of inorganic solid peroxide |
| CN105036293A (en) * | 2015-08-27 | 2015-11-11 | 哈尔滨工业大学 | Method for removing organic pollutants in water by ferrate reinforced ozone oxidation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62123025A (en) * | 1985-11-25 | 1987-06-04 | Nippon Zeon Co Ltd | Production of powdery composition containing iron compound |
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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 |
| CN101088926A (en) * | 2006-06-12 | 2007-12-19 | 深圳职业技术学院 | Combined water-treating farrate-fenton reagent process |
| CN103553203A (en) * | 2013-11-20 | 2014-02-05 | 哈尔滨理工大学 | Method for treating reverse osmosis concentrated solution by using singlet oxygen produced from peroxymonosulfate under induction of inorganic solid peroxide |
| CN105036293A (en) * | 2015-08-27 | 2015-11-11 | 哈尔滨工业大学 | Method for removing organic pollutants in water by ferrate reinforced ozone oxidation |
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