CN108190965A - A kind of preparation method of Na2Fe04 solution - Google Patents
A kind of preparation method of Na2Fe04 solution Download PDFInfo
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- CN108190965A CN108190965A CN201810307904.7A CN201810307904A CN108190965A CN 108190965 A CN108190965 A CN 108190965A CN 201810307904 A CN201810307904 A CN 201810307904A CN 108190965 A CN108190965 A CN 108190965A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0081—Mixed oxides or hydroxides containing iron in unusual valence state [IV, V, VI]
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Abstract
The present invention relates to Water Treatment pharmaceutical formulation techniques fields, refer in particular to a kind of preparation method of Na2Fe04 solution, and preparation process is as follows；Step 1：A certain amount of liquor natrii hypochloritis is added in reactor, then sodium hydroxide is added in or potassium hydroxide, controlling reaction temperature obtains the sodium hypochlorite aqueous slkali of saturation between 15~40 degrees Celsius；Step 2：Trivalent iron salt is added in the sodium hypochlorite aqueous slkali obtained into step 1, is heated, and carry out ultrasonic oscillation；Step 3：Stabilizer, 30~120 minutes reaction time are added in into reactor；Step 4：The solution that step 3 obtains is centrifuged, takes supernatant, obtains Na2Fe04 solution.The present invention improves reaction efficiency to the maximum extent, is assisted in building-up process by the ultrasonic echography of appropriate power, improves reaction efficiency.Na2Fe04 stability of solution prepared by the present invention is good, and yield is high, is easy to industrialized production, is easy to that onsite application is prepared in situ.
Description
Technical field
The present invention relates to Water Treatment pharmaceutical formulation techniques fields, refer in particular to a kind of preparation side of Na2Fe04 solution
Method.
Background technology
The special chemical property of Na2Fe04, it has very high application value in water treatment procedure, be it is a kind of collection disinfection,
High-efficiency multi-function chemistry in water treatment medicament being condensated as a whole, having no toxic side effect is aoxidized, flocculated, adsorbed and helped, is had important
Research and development and popularizing application prospect.Na2Fe04 is the green disinfectant that scientists are generally acknowledged, ferro element in Na2Fe04
For positive sexavalence, there is very strong oxidisability, it is soluble in water to discharge a large amount of elemental oxygen, so as to effectively kill in water
Germ and virus.At the same time, the hydroxide three-iron of nascent state itself is reduced into, this is a kind of inorganic flocculation best in quality
Agent can efficiently remove the fine suspended matter in water.But since the yield of Na2Fe04 is extremely low, and it is unstable not easy to maintain,
Improving its yield becomes the difficult point that researcher pays close attention to jointly, and this technology is as starting point, to improve its concentration and production
Rate is target.
The method for preparing Na2Fe04 at present is broadly divided into three kinds, high-temperature oxidation, hypochlorite oxidation method and electrolysis.
High-temperature oxidation is by peroxide and iron containing compounds or iron simple substance, and high-temperature fusion reaction occurs in the presence of caustic alkali and comes
It preparing, such method prepares Na2Fe04, and the rate of recovery and conversion ratio are higher, but chemical reagent consumption is big, and required reaction temperature is high,
Container corrosion is serious, dangerous big, is seldom prepared at present using this method.The advantages of electrolysis is that reaction is easy to control, former
Material consumption is few, environmentally safe etc., but its most important shortcoming is that current efficiency is low, side reaction is more, prepared ferric acid
Sodium solution concentration is very low, and purification is complicated, meanwhile, itself passivation phenomenon can occur for electrode, then the strong oxidizing property for having Na2Fe04 makes
Own is decomposed, and causes electrolysis synthesized high iron acid sodium that cannot reach the requirement of industrialized production, although electrolysis operates
It is relatively simple, but it is its critical defect that product design is low.Hypochlorite oxidation method synthesized high iron acid sodium is mainly characterized by：After purification
The yield of Na2Fe04, purity it is relatively high, but processing step is complicated, and manufacturing cost is high, and yield is relatively low, prepared high ferro
Acid sodium solution stability is poor, and storage time is short, and worker and environment are generated not to chlorine involved in most building-up processes
Sharp factor is inevitable.
Up to now, it there is no a kind of preparation process for being suitable for industrialization large-scale production ferrate so that ferric acid
Salt still cannot be widely applied to every field, therefore carry out the research and development of ferrate preparation process with highly important
Meaning.
Invention content
The technical problem to be solved in the present invention is to provide one kind in the case where improving Na2Fe04 yield and purity, simplify
Processing step, the preparation method for reducing manufacturing cost, the Na2Fe04 solution for removing influence of the chlorine to synthesis technology.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that：A kind of preparation side of Na2Fe04 solution
Method, preparation process are as follows；
Step 1：A certain amount of liquor natrii hypochloritis is added in reactor, then adds in sodium hydroxide or potassium hydroxide, control
Reaction temperature processed obtains the sodium hypochlorite aqueous slkali of saturation between 15~40 degrees Celsius；
Step 2：Trivalent iron salt is added in the sodium hypochlorite aqueous slkali obtained into step 1, is heated, and carry out ultrasonic oscillation；
Step 3：Stabilizer, 30~120 minutes reaction time are added in into reactor；
Step 4：The solution that step 3 obtains is centrifuged, takes supernatant, obtains Na2Fe04 solution.
Preferably, in the step 1：A certain amount of liquor natrii hypochloritis is added in reactor, by several times in fixation
Time in add in a certain amount of sodium hydroxide or potassium hydroxide, by water-bath controlling reaction temperature 15~40 degrees Celsius it
Between, obtain the sodium hypochlorite aqueous slkali of saturation.
Preferably, in the step 1：40~80 milliliters of liquor natrii hypochloritis is added in reactor, Ran Hou
In 20~60 minutes, 16~40 grams of sodium hydroxide or potassium hydroxide are equally divided into 3~6 times, added within 4~8 minutes per minor tick
Enter to reactor, by between water-bath controlling reaction temperature again 15~40 degrees Celsius, obtaining the sodium hypochlorite aqueous slkali of saturation.
Preferably, the concentration accounting that sodium hydroxide or potassium hydroxide are added in the step 1 is 20%~40%.
Preferably, the trivalent iron salt is one or several kinds of mixtures in ferric nitrate, ferric sulfate and iron chloride.
Preferably, in the step 2, the molar ratio of trivalent iron salt and sodium hypochlorite aqueous slkali is 1:1.5~3.
Preferably, in the step 2：Trivalent iron salt is at the uniform velocity added dropwise in sodium hypochlorite aqueous slkali using constant flow pump,
Heating water bath, 30~60 degrees Celsius of controlling reaction temperature, the reaction time is 30~300 minutes, while starts ultrasonic oscillation.
Preferably, it is 30~300 minutes that the ultrasonic oscillation, which continues running time, and ultrasonic frequency is 20~50 kilo hertzs
Hereby.
Preferably, the stabilizer is sodium metasilicate, guar gum, sodium metasilicate, calcium hypochlorite, potassium silicate, potassium methyl silicate
With one or several kinds of mixtures in cyclodextrin.
Preferably, in the step 3：Stabilizer is added in, it is 30~120 minutes to be stirred to react the time.
Preferably, the centrifugation rate of the centrifugation in the step 4 is 2000~5000 rpms, and centrifugation time is
5~30 minutes.
The beneficial effects of the present invention are：A kind of preparation method of Na2Fe04 solution is provided, the present invention is to greatest extent
Ground improves reaction efficiency, is assisted in building-up process by the ultrasonic echography of appropriate power, improves reaction efficiency.It adds in few
After measuring compound stabilizer agent, it can effectively inhibit the decomposition of ferrate.Na2Fe04 stability of solution prepared by the present invention is good, production
Rate is high, is easy to industrialized production, is easy to that onsite application is prepared in situ, adds in sonic oscillation, reacts and carried out toward beneficial direction, can be very
The concentration of good raising Na2Fe04, gained Na2Fe04 yield, concentration are relatively high, and raw material availability is high, and manufacturing cost is low,
Chlorine is not generated in building-up process, without heating, charging is simple, and environmentally safe, the Na2Fe04 solution of generation can be straight
It connects and is added in river and sewage, unharmful substance generates, and flocculating effect is splendid.The Na2Fe04 produced is sexavalence molysite, tool
There is very strong oxidisability, it is soluble in water to discharge a large amount of elemental oxygen, so as to effectively kill germ and the virus in water.
At the same time, itself it is reduced into the Fe of nascent state（OH）3, this is a kind of inorganic flocculating agent best in quality, can efficiently be removed
The fine suspended matter in water is removed, for handling the exceeded sewage such as COD, ammonia nitrogen.
Specific embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
A kind of preparation method of Na2Fe04 solution, preparation process are as follows；
Step 1：A certain amount of liquor natrii hypochloritis is added in reactor, then adds in sodium hydroxide or potassium hydroxide, control
Reaction temperature processed obtains the sodium hypochlorite aqueous slkali of saturation between 15~40 degrees Celsius；
Step 2：Trivalent iron salt is added in the sodium hypochlorite aqueous slkali obtained into step 1, is heated, and carry out ultrasonic oscillation；
Step 3：Stabilizer, 30~120 minutes reaction time are added in into reactor；
Step 4：The solution that step 3 obtains is centrifuged, takes supernatant, obtains Na2Fe04 solution.
The preparation method of the Na2Fe04 solution of the present embodiment, improves reaction efficiency, in building-up process to the maximum extent
It is assisted by the ultrasonic echography of appropriate power, improves reaction efficiency.After adding in a small amount of compound stabilizer agent, can effectively it inhibit
The decomposition of ferrate.Na2Fe04 stability of solution prepared by the present invention is good, and yield is high, is easy to industrialized production, is easy to existing
Field prepares onsite application, adds in sonic oscillation, reacts and is carried out toward beneficial direction, can improve the concentration of Na2Fe04, institute well
It is relatively high to obtain Na2Fe04 yield, concentration, raw material availability is high, and manufacturing cost is low, and chlorine is not generated in building-up process, without
Heating, charging is simple, and environmentally safe, the Na2Fe04 solution of generation can be added directly into river and sewage, and nothing has
Evil substance generation, flocculating effect are splendid.The Na2Fe04 produced is sexavalence molysite, has very strong oxidisability, energy soluble in water
A large amount of elemental oxygen is discharged, so as to effectively kill germ and the virus in water.At the same time, itself is reduced into new life
The Fe of state（OH）3, this is a kind of inorganic flocculating agent best in quality, the fine suspended matter in water can be efficiently removed, for locating
Manage the exceeded sewage such as COD, ammonia nitrogen.
Embodiment one：
First prepare the ferrum sulfuricum oxydatum solutum of 0.25mol/l；Liquor natrii hypochloritis's pipette of pure concentration will be analyzed, 40ml is moved and enters four
In mouth round-bottomed flask；The sodium hydroxide of 16~19g is weighed, opens blender, slow the pouring at the uniform velocity by the sodium hydroxide weighed
In round-bottomed flask, plug is clogged, after liquor natrii hypochloritis and sodium hydroxide solution temperature reach room temperature, opens water bath with thermostatic control
Pot, temperature is respectively 20~30 degrees Celsius, then 30~40ml is taken to add in constant flow pump the ferrum sulfuricum oxydatum solutum prepared, treats practical temperature
Degree reach set temperature when, open constant flow pump, start slowly at the uniform velocity be added to sodium hydroxide and the mixing of liquor natrii hypochloritis
In solution, while supersonic oscillations are opened, power is 50~100W, and supersonic frequency is 20~40KHz, is reacted 30~60 minutes,
0.2~0.4 gram of stabilizer sodium metasilicate is added in, the reaction was continued 30~60 minutes, takes out solution, is fitted into centrifuge tube, is centrifuged
4000rad/min, centrifuge 5min, after supernatant is poured into quartz colorimetric utensil, be put into ultraviolet specrophotometer, quantified
Analysis.
Embodiment two：
First prepare the ferric chloride solution of 0.25mol/l；Liquor natrii hypochloritis's pipette of pure concentration will be analyzed, 40ml is moved and enters four
In mouth round-bottomed flask；Weigh the sodium hydroxide of 9~12g, open blender, by the sodium hydroxide weighed slowly at the uniform velocity pour into circle
In the flask of bottom, plug is clogged, after liquor natrii hypochloritis and sodium hydroxide solution temperature reach room temperature, opens thermostat water bath,
Temperature is respectively 40~50 degrees Celsius, then 30~40ml is taken to add in constant flow pump the ferric chloride solution prepared, treats actual temperature
Reach set temperature when, open constant flow pump, start slowly at the uniform velocity be added to sodium hydroxide and the mixing of liquor natrii hypochloritis is molten
In liquid, while supersonic oscillations are opened, power is 100~150W, and supersonic frequency is 40~60KHz, reacts 60~80 minutes, adds
Enter 0.2~0.4 gram of stabilizer potassium silicate, the reaction was continued 30~60 minutes, takes out solution, is fitted into centrifuge tube, is centrifuged
4000rad/min, centrifuge 5min, after supernatant is poured into quartz colorimetric utensil, be put into ultraviolet specrophotometer, quantified
Analysis.
The Na2Fe04 solution that embodiment one and embodiment two are prepared carries out the data comparison result after quantitative analysis
It is as follows：
First, influence of the Na2Fe04 dosage to NH_3-N treating effect
A concentration of 67.25mg/l ammonia nitrogens are prepared with the ammonium chloride of 0.2635g, after being completely dissolved, 100ml is measured with graduated cylinder and pours into
In the beaker of 200ml；1ml, 2ml, 3ml, 4ml, 5ml and 6ml are taken as respectively with the Na2Fe04 solution of 0.02492mol/l to add
Enter into the beaker for filling ammonia nitrogen solution, 120min is placed after stirring and surveys an ammonia nitrogen value, carry out data processing and obtain following table
Lattice：
Table 1：Influence of the Na2Fe04 dosage difference to ammonia nitrogen（120min）
By Na2Fe04 add 120min after experimental data table it can be seen from when adding 3ml, the effect of Na2Fe04 is bright
Aobvious, removal effect has reached 81.95%, and when adding Na2Fe04 4ml, removal effect is up to 97.37%, and effect is extremely apparent.
2nd, influence of the Na2Fe04 to various concentration ammonia nitrogen and the Na2Fe04 without ultrasonic wave assisted reaction are to ammonia nitrogen
It influences
With chloride solid, the ammonia nitrogen solution of various concentration is respectively configured out, ammonia nitrogen concentration is respectively 45.30 mg/l, 53.00
Mg/l, 62.10 mg/l, 72.10 mg/l and 81.50mg/l, put into further according to 5ml Na2Fe04s in 100ml ammonia nitrogen solutions
Add ratio, be added separately in ammonia nitrogen solution, after stirring stand 60min be measured thus carry out data processing obtain with
Lower table：
Table 2：Influence of the Na2Fe04 to various concentration ammonia nitrogen
Table 3：Influence of the Na2Fe04 of non-ultrasonic wave assisted reaction to ammonia nitrogen
The Na2Fe04 processing ammonia nitrogen effect that ultrasound obtains later is better than the Na2Fe04 processing ammonia nitrogen effect that ultrasound does not obtain
4%-8%。
By above table data analysis it can be seen that, the preparation method of the Na2Fe04 solution of the present embodiment, to greatest extent
Ground improves reaction efficiency, is assisted in building-up process by the ultrasonic echography of appropriate power, improves reaction efficiency.It adds in few
After measuring compound stabilizer agent, it can effectively inhibit the decomposition of ferrate.Na2Fe04 stability of solution prepared by the present invention is good, production
Rate is high, is easy to industrialized production, is easy to that onsite application is prepared in situ.
It should be noted that description purpose is only used for if any term " first ", " second ", and it is not intended that instruction or dark
Show relative importance or the implicit quantity for indicating technical characteristic.Define " first " as a result, " second " feature can be expressed or
Implicit to include one or more this feature, in the present description, " several " are meant that two or more, unless separately
There is clearly specific limit.
In the present invention, except as otherwise clear stipulaties and restriction, should make if any term " assembling ", " connected ", " connection " term
Broad sense goes to understand, for example, it may be being fixedly connected or being detachably connected or be integrally connected；Can also be that machinery connects
It connects；It can be directly connected or be connected by intermediary, can be connected inside two elements.For ability
For the those of ordinary skill of domain, the concrete meaning of above-mentioned term in the present invention can be understood as the case may be.
Embodiment described above only expresses several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of Na2Fe04 solution, it is characterised in that：Preparation process is as follows；
Step 1：A certain amount of liquor natrii hypochloritis is added in reactor, then adds in sodium hydroxide or potassium hydroxide, control
Reaction temperature processed obtains the sodium hypochlorite aqueous slkali of saturation between 15~40 degrees Celsius；
Step 2：Trivalent iron salt is added in the sodium hypochlorite aqueous slkali obtained into step 1, is heated, and carry out ultrasonic oscillation；
Step 3：Stabilizer, 30~120 minutes reaction time are added in into reactor；
Step 4：The solution that step 3 obtains is centrifuged, takes supernatant, obtains Na2Fe04 solution.
2. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：In the step 1：By one
Quantitative liquor natrii hypochloritis is added in reactor, interior at a fixed time by several times to add in a certain amount of sodium hydroxide or hydrogen-oxygen
Change potassium, by water-bath controlling reaction temperature between 15~40 degrees Celsius, obtain the sodium hypochlorite aqueous slkali of saturation.
3. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：Hydrogen is added in the step 1
The concentration accounting of sodium oxide molybdena or potassium hydroxide is 20%~40%.
4. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：The trivalent iron salt is nitric acid
One or several kinds of mixtures in iron, ferric sulfate and iron chloride.
5. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：In the step 2, trivalent
The molar ratio of molysite and sodium hypochlorite aqueous slkali is 1:1.5~3.
6. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：In the step 2：It utilizes
Trivalent iron salt is at the uniform velocity added dropwise in sodium hypochlorite aqueous slkali by constant flow pump, heating water bath, 30~60 degrees Celsius of controlling reaction temperature,
Reaction time is 30~300 minutes, while starts ultrasonic oscillation.
7. the preparation method of the Na2Fe04 solution according to claim 1 or 6, it is characterised in that：The ultrasonic oscillation
It is 30~300 minutes to continue running time, and ultrasonic frequency is 20~50 kHz.
8. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：The stabilizer is silicic acid
One or several kinds of mixtures in sodium, guar gum, sodium metasilicate, calcium hypochlorite, potassium silicate, potassium methyl silicate and cyclodextrin.
9. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：In the step 3：It adds in
Stabilizer, it is 30~120 minutes to be stirred to react the time.
10. the preparation method of Na2Fe04 solution according to claim 1, it is characterised in that：Centrifugation in the step 4
The centrifugation rate of separation is 2000~5000 rpms, and centrifugation time is 5~30 minutes.
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| CN201810307904.7A CN108190965A (en) | 2018-04-08 | 2018-04-08 | A kind of preparation method of Na2Fe04 solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114853129A (en) * | 2022-05-23 | 2022-08-05 | 常州清流环保科技有限公司 | In-situ composite aluminum ferrite water treatment agent and preparation method and application method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318707A (en) * | 2008-07-01 | 2008-12-10 | 上海大学 | Method for preparing steady composite potassium ferrate solution |
| CN103449528A (en) * | 2013-08-09 | 2013-12-18 | 华南理工大学 | Method for preparing ferrate through ultrasonic activation |
-
2018
- 2018-04-08 CN CN201810307904.7A patent/CN108190965A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318707A (en) * | 2008-07-01 | 2008-12-10 | 上海大学 | Method for preparing steady composite potassium ferrate solution |
| CN103449528A (en) * | 2013-08-09 | 2013-12-18 | 华南理工大学 | Method for preparing ferrate through ultrasonic activation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114853129A (en) * | 2022-05-23 | 2022-08-05 | 常州清流环保科技有限公司 | In-situ composite aluminum ferrite water treatment agent and preparation method and application method thereof |
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Application publication date: 20180622 |